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Superalloys

for Industry Applications


Edited by Sinem Cevik
SUPERALLOYS FOR
INDUSTRY APPLICATIONS

Edited by Sinem Cevik


Superalloys for Industry Applications
http://dx.doi.org/10.5772/65570
Edited by Sinem Cevik

Contributors
Sgk Manikandan, M Kamaraj, D Sivakumar, Facundo Almeraya-Calderon, Manuel Alejandro Lira Martinez, Taboada
Jorge, José Cabral, Patricia Zambrano-Robledo, Citlalli Gaona, Francisco Estupiñan, Yongbo Wu, Qiang Wang, Sisi Li,
Dong Lu, Nageswara Rao Muktinutalapati, Arivazhagan Natarajan, Arivarasu M, Mohieddine Benghersallah, Sutter
Guy, List Gautier, Lavinia Cosmina Ardelean, Lucien Reclaru, Cristina Maria Bortun, Brandusa Ghiban

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Meet the editor

Dr. Sinem Çevik is currently an assistant professor in


Metallurgical and Materials Engineering at the Ondokuz
Mayis University, Samsun, Turkey. She has a particular
interest in the areas of superalloys, welding, solidifi-
cation cracks, corrosion/oxidation of metals and their
alloys, electrochemistry, ceramics, coatings, and thin
films. Her PhD studies are related to the evaluation of
HAZ microfissures of superalloys. Her MSc thesis on anodic reactions of
tungsten was submitted in 2003. She graduated from the Department of
Metallurgical and Materials Engineering, METU, Turkey, with a gradu-
ation thesis on different welding techniques. She performed research on
piezoelectricity of materials at the Penn State University, USA, in 2004. She
also joined the MEMS group at the University of the West of Scotland with
a project on AlN piezoelectric thin films in 2008. At present, she has pub-
lished 10 papers, 35 proceedings, and 3 book chapters. She also worked on
different international and national projects.
Contents

Preface VII

Chapter 1 Laves Phase in Alloy 718 Fusion Zone 1


S.G.K. Manikandan, D. Sivakumar and M. Kamaraj

Chapter 2 High-Temperature Oxidation of Superalloy C-263 of Rings for


Aircraft Engines 15
Citlalli Gaona Tiburcio, Alejandro Lira Martinez, Jorge Taboada
Solis, Patricia Zambrano Robledo, Francisco Estupiñán López, Jose
Cabral Miramontes and Facunda Almeraya Calderón

Chapter 3 Hot Corrosion of Superalloys in Boilers for Ultra-Supercritical


Power Plants 29
Nageswara Rao Muktinutalapati, Arivazhagan Natarajan and
Moganraj Arivarasu

Chapter 4 Ultrasonic Assisted Machining of Nickel-Based Superalloy


Inconel 718 43
Yongbo Wu, Qiang Wang, Sisi Li and Dong Lu

Chapter 5 Dry High Speed Orthogonal Turning of Titanium Alloy Wear


Evolution and Chip Morphology 65
Mohieddine Benghersallah, Lakhdar Boulanouar, Gautier List and
Guy Sutter

Chapter 6 Laser Welding of Different Dental Alloys 85


Lavinia Cosmina Ardelean, Lucien Reclaru, Cristina Maria Bortun
and Brandusa Ghiban
Preface

Innovations in the aerospace and aircraft industry have thrown light on building the fu‐
ture’s engineering architecture in today’s globalized world, where technology is an indis‐
pensable part of our lives. On the basis of the aviation sector, innovations in the materials
used in aircraft parts have to be continuously maintained its actuality. At this point, superal‐
loys have been proceeding in the way to become a material that aerospace and defense in‐
dustries never replace of any other material when combining its good mechanical
properties, easy machinability, and low cost. In spite of their superior properties, these ma‐
terials suffer from wear, tear, and crack in order to be exposed to the elevated working tem‐
peratures and the harsh operating environments in service.
In Within the scope of this book, the superalloys usually used in gas turbine engine parts are
reviewed. Improvements of materials used in aircraft gas turbine engines, which constitute
50% of total aircraft weight, must be protected continuously. The utilization of superalloys
in the aerospace and defense industries cannot be ignored because of their excellent corro‐
sion and oxidation resistance, high strength, and long creep life at elevated temperatures.
This book provides information on the interaction between the microstructure of alloys and
their mechanical properties and also the position of superalloys in the manufacturing indus‐
try. Topics cover the minimization of the formation of microsegregation and detrimental
phases in the GTA welding of superalloys, oxidation kinetics of nickel-based superalloys
used in the manufacture of rings for aircraft engines, a review of the work done over the last
two decades to understand the hot corrosion behavior of superalloys used in advanced coal-
based power plants, ultrasonic-assisted machining of Inconel 718, dry high-speed turning of
Ti-6Al-4V titanium alloy, and laser welding in dentistry.
This book serves as a guide to those interested in superalloys and materials, their properties,
techniques of manufacturing, application areas, and so on. Thus, the engineers in the indus‐
try, the students in colleges and universities, and the lecturers giving courses at both under‐
graduate and postgraduate levels can use this book as an international reference.
The book “Superalloys for Industry Applications” consists of contributions by scientists and
engineers who are experienced in the production, design, and analysis of materials from all
around the world. We hope that this book will be an irreplaceable source of study for manu‐
facturing, degradation mechanisms, and reliability of superalloys.

Sinem Çevik
Ondokuz Mayis University, Turkey
DOI: 10.5772/intechopen.70325

Provisional chapter

Chapter 1
Laves Phase in Alloy 718 Fusion Zone
Laves Phase in Alloy 718 Fusion Zone
S.G.K. Manikandan, D. Sivakumar and
M. Kamaraj
S.G.K. Manikandan, D. Sivakumar and M. Kamaraj
Additional information is available at the end of the chapter
Additional information is available at the end of the chapter

http://dx.doi.org/10.5772/intechopen.70325

Abstract

The gas tungsten arc (GTA) welded fusion zone of alloy 718 has been well investigated
on the formation of interdendritic Laves phase. This article deals with the various pro-
cess control methodologies for minimizing the microsegregation and Laves phase such
as the enhanced weld cooling rate in GTA welding (GTAW) process and modification in
weld metal chemistry. Even though the high energy density welding processes such as
electron beam (EB) and laser beam (LB) welding techniques are proven in minimizing
the microsegregation and Laves phase, the requirement of conventional GTA welding
process still exists in the aerospace industry due to the complex shapes of the compo-
nents and the inaccessible conditions for executing the welding process. The enhance-
ment in the weld cooling rate and modified weld metal chemistry resulted in the refined
fusion zone microstructure and reduced microsegregation. Enhanced weld efficiency on
ultimate tensile strength (UTS) and 0.2% YS at 25°C was observed to the tune of 85 to
93% by employing cryogenic cooling in GTA welding process. Similar improvement in
weld efficiency at 650°C was observed. However, the evaluated weld efficiencies with
cryogenically cooled weld metal were marginally lower than the previous works in EB
and LB welds only by 2–3%.

Keywords: Laves phase, alloy 718, GTAW, X-ray diffraction, tensile strength,
microsegregation

1. Introduction

Alloy 718 is extensively used in the high-temperature systems of cryogenic rocket engines
in Indian launch vehicles. Use of Nb as age hardener in place of Al or Ti in alloy 718 elimi-
nated the problem of strain age cracking, but resulted in the formation of brittle inter-
connected Laves phase during welding [1] which are the favorable sites for easy crack

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2 Superalloys for Industry Applications

initiation and propagation. This affects the aging response, tensile properties, and duc-
tility of the welded components [2]. Hence control on the morphology and continuity of
the Laves phase during solidification was found to be essential. Published information on
the control of Laves phase formation in alloy 718 welds is limited to autogenous welds of
gas tungsten arc welding (GTAW), electron beam welding (EBW) and laser beam welding
(LBW) [3], current pulsing with simple square waveform and magnetic arc oscillation in
GTAW [4]. It was concluded that the faster cooling rate reduced the level of interdendritic
Nb segregation and amount of Laves phase. But high energy density processes cannot be
adopted in rocket engines due to the complex shapes and highly inaccessible areas. Zhang
and Liu reported that the cooling rate was enhanced with the higher growth rate and steep
temperature gradient [5]. Hence pulse current manual GTA welding process is relied upon
with limited options such as modified pulse waveform [6] and helium shielding gas to
enhance the cooling rate and minimize the segregation. Their effect on formation of Laves
phase and microsegregation of niobium in alloy 718 fusion zone has been discussed.
The influence of cryogenic coolants on microstructures was investigated earlier [6, 7]. Hence
rapid heat dissipation dynamics using liquid nitrogen was studied in the present work during
manual GTA welding process for further enhancing the weld cooling rate. Filler metals with
significantly different compositions from that of the base material composition were used to
minimize Laves phase in some of the welding applications [8]. This was the driving force for
studying the solidification behavior of alloy 718 fusion zone welded with high Mo (16 wt%)
filler metal, even though it was well established by various researchers [9, 10]. The present study
also describes the influence of hybrid pulsing in the range of 500–2000 Hz on the fusion zone
microstructure and interdendritic segregation of alloy 718 welds. The effects of pulse frequency
have been analyzed through solidification parameters and related mechanisms on the interden-
dritic segregation in alloy 718 fusion zone. In view of the above, an attempt has been made in the
present study to evaluate the effectiveness of cooling techniques in controlling the formation of
Laves phase and the high-temperature mechanical properties in alloy 718 GTA welds.

Primarily, this chapter deals with the control of laves phase formation in the fusion zones of
alloy 718 weldments by enhanced weld cooling rate through modified pulse current wave-
form and shielding gases (Argon and Helium) in GTA welding process and change of weld
metal chemistry using solid solution (FM1) and matching composition/age-hardenable (FM2)
filler metal. Secondly, the mechanical properties at room temperature and elevated tempera-
tures have been correlated to the Laves phase in the weld fusion zone of alloy 718.

2. Materials and methods

The specimens were prepared from alloy 718 sheets of 2 mm thick (for welding experiments)
and 3 mm (for solidification experiments) in 980°C solution treated condition using gas tungsten
arc welding process. The solidification experiments were conducted in autogenous mode GTAW
with thermocouples welded at the center of the weld and adjacent to the fusion zone in a 5 × 5
array in order to obtain both longitudinal and transverse temperature distribution. The details
of the chemical composition for base material and filler metal are given in Table 1. The weld
Laves Phase in Alloy 718 Fusion Zone 3
http://dx.doi.org/10.5772/intechopen.70325

Element C Mn Si Cr Fe Mo Nb + Ta Ti Al Cu Ni
Base metal 0.05 0.11 0.1 18.2 19.8 2.8 5 1 0.6 0.03 Bal.

FM1 0.05 2 0.5 16 5 16 - - - - Bal.

FM2 0.08 0.55 0.4 21 16 3.3 5.5 1.15 0.8 0.3 Bal.

Table 1. Chemical composition of base metal and filler metals (in wt%).

parameters for square butt joints with an optimized heat input value of 0.75–0.77 kJ/mm were
employed. The conventional copper heat sink and liquid nitrogen were used for the external
cooling. Similarly, modified pulse wave form (constant current, compound current, and hybrid
pulsing) with argon and helium shielding gas were employed for the in-process cooling.
Welded samples were subjected to the aging treatment as per AMS 5596 K after 100% X-ray
radiography and dye penetrant test. The samples were etched using Kalling’s reagent and
the weld microstructures and elemental mapping were obtained with field emission gun
scanning electron microscope (FE-SEM) with an acceleration voltage of 20 kV. The elemental
mapping of Nb in the dendritic and interdendritic zones was carried out in a thermal field
emission electron microprobe (EPM JXA-8530F) over the metallographically prepared and
unetched specimens with an acceleration voltage of 15 kV.
Electron diffraction studies were carried out with 3 mm diameter and 90 μm thickness discs of
the as-welded and the direct-aged fusion zone using Jeol make transmission electron micro-
scope (TEM) equipment. Differential thermal analysis was conducted to finalize the heating
rate among the three heating rates of 5, 10, and 20°C/min using SII 6300 EXSTAR with a
sample weight of 0.02 ± 0.0005 g in an argon atmosphere at a flow rate of 0.2 l/min. Differential
scanning calorimetric analysis was performed on a SETARAM LABSYS 1600 heat flux type
DSC instrument to measure eutectic type reaction temperatures with an optimized heating
rate of 10°C/min and a cooling rate of 20°C/min. The tensile test of the specimen at 25 and
650°C were conducted at a strain rate of 1 × 10−3 s−1 as per ASTM E8 and E21-09, respectively.
An air circulating furnace with accuracy in temperature of ±3°C was used for conducting the
650°C tensile test. The fracture morphology was studied using scanning electron microscope.

3. Microstructural characterization of fusion zone

The conventionally cooled GTA welded fusion zone microstructure using argon shielded con-
stant current technique (weld cooling rate: 40°C/s) revealed a mixed dendritic structure con-
sisting of columnar and/or elongated dendritic and equiaxed dendritic structures as shown
in Figure 1(a). The fusion zone exhibited coarse columnar dendrites from the fusion line to
the middle of the fusion zone due to the experimentally measured longitudinal temperature
gradient in the order of −39.26°C/mm along the welding direction.
But the fusion zone of compound current pulse with conventional cooling measured a weld
cooling rate of 394°C/s, the corresponding fusion zone exhibited a finer equiaxed dendritic
structure as shown in Figure 1(c). The transition from columnar-to-equiaxed (CET) was
4 Superalloys for Industry Applications

Figure 1. Micrographs of conventionally cooled fusion zones (a, c), heat affected zones (b, d) and cryogenically cooled
fusion zone (e), heat affected zone (f) using constant current (40°C/s) and compound current pulse technique (394,
510°C/s), respectively.

shifted away from the center of the fusion zone by the enhanced longitudinal temperature
gradient existed ahead of the columnar front of the order of −195.16°C/mm. The base material
grains were recrystallized and epitaxial growth was initiated with finer grains which led to
the formation of fine columnar dendritic structure near to the heat affected zone as evidenced
in Figure 1(d).

Similar observations were made on the microstructures of the cryogenically cooled (liquid
nitrogen) GTA welded fusion zone with finer equiaxed dendritic structures than that of the
conventional cooling method as shown in Figure 1(e) for the same set of welding variables
(as used for the weld cooling rate of 394°C/s). The refinement of fusion zone microstructure
was due to the imposed cooling rate. The extent of refinement of the fusion zone microstruc-
ture was also enhanced till the middle of the fusion zone. Certain regions in the middle of
the fusion zone revealed the dendrite to cellular transition as shown in Figure 1(e) by the
degeneration of side branches through dendrite arm remelting mechanism due to the varia-
tion in the morphology parameter (temperature gradient/growth rate—G/R). As presented in
Figures 1(b), (d), and (f), and 2(e) and (f), microfissures were not observed in the heat affected
zone of both the conventionally cooled and liquid nitrogen-cooled weldments. The base mate-
rial grains were coarsened in the lowest weld cooling rate (40°C/s). The grain growth was
limited with the enhanced cooling rate as shown in Figure 2(f), especially in the liquid nitro-
gen-cooled weldments through the reduced transverse temperature gradient by the impinge-
ment of cold nitrogen vapor.
The SE micrographs of conventionally cooled fusion zone exhibited a thick and continuous
interdendritic Laves network as shown in Figure 2(a) due to the increased time at tempera-
ture parameter and reduced longitudinal temperature gradient (−39.26°C/mm) which led to a
Laves Phase in Alloy 718 Fusion Zone 5
http://dx.doi.org/10.5772/intechopen.70325

Figure 2. SE micrographs of (a, b) conventionally cooled, (c, d) liquid nitrogen-cooled GTA welded fusion zone and (e, f)
respective heat affected zone.

lower weld cooling rate (40°C/s) and higher solidification time resulted an enhanced microse-
gregation. Figure 3 details about the quantitative elemental analyses of GTA weld fusion zone
for the six weld cooling rates (40, 80, 394, 265, 362, and 510°C/s).
The quantitative elemental analysis exhibited that microsegregation was reduced with
increased weld cooling rate. This was revealed by the increase of niobium content in the
dendritic regions of both the FM1 and FM2 fusion zone with the weld cooling rate. As shown
in Figure 2(a), the Nb rich zones present in the FM2 fusion zone (40°C/s) exhibited rela-
tively higher niobium content in the dendritic region due to the pickup from the adjacent
zones. As the iron content increased in the dendrite, more of niobium was rejected into the
interdendritic regions due to the limited solubility of Nb which resulted in the increased
microsegregation [8]. The fusion zone (394°C/s) microstructure consisted of γ-matrix with
clear solidification grain boundaries and discrete Laves particles in the interdendritic regions
as in Figure 2(b).
The microsegregation was significantly reduced by employing the in-process cooling method
such as compound current pulse and helium shielding gas which enhanced the longitudinal
temperature gradient and growth rate. Thus the fusion zone microstructure was refined. The
liquid nitrogen-cooled fusion zone microstructures for the constant current (265°C/s) mode
revealed finer and disconnected interdendritic Laves particles as shown in Figure 2(c). As
the weld cooling rate was increased to 510°C/s by employing the compound current pulse
mode, the microstructure of the fusion zone was further refined and resulted with relatively
finer Laves particles as shown in Figure 2(d). Since the interdendritic microsegregation was
6 Superalloys for Industry Applications

Figure 3. Elemental analysis of alloy 718 fusion zone using FE-SEM/EDS.

reduced, the dendrite was enriched with niobium for the higher weld cooling rates. It was
observed that Nb concentration in FM2 fusion zone was comparable to the base material com-
position at higher weld cooling rate (510°C/s). As the iron content was decreasing (kFe =0.98
to 0.76 for FM1 and kFe = 1 to 0.63 for FM2) with the increase in weld cooling rate as given in
Figure 3 which aided in reducing the microsegregation. In addition, an increase in nickel con-
tent at higher weld cooling rate (510°C/s) was observed. This helped in retaining the Nb con-
tent in the matrix and thereby the concentration of Nb in the dendritic regions was increased.

As discussed previously, the decrease of iron content in the dendrite core with the increased
weld cooling rate indicated that the weld dilution levels were reduced for the maximum cool-
ing rate employed in the present study. The present study took advantage of the modified
pulse waveform and the helium shielding gas which aided in constricting the arc; thereby,
the weld dilution levels were minimized in the present study. Hence the solubility of nio-
bium and molybdenum were increased because of the reduced iron content in γ matrix and
the resultant interdendritic segregation was also reduced. In our present study, the distribu-
tion trend of elements in the fusion zone was comparable with the previous research work
[8]. However, the localized niobium rich zones in FM2 fusion zone modified the elemental
distribution trend of niobium at lowest weld cooling rate. The HAZ of both the weldments
were free from microfissures and grain boundary liquation as shown in Figure 2(e) and (f)
due to the balanced transverse temperature gradient because of the longitudinal holes on the
top of the cooling system with an angle of attack for cooling the HAZ region. The interden-
dritic phases in the fusion zone were found to be of C14 type Laves phases with hcp crystal
structure (a = 0.4831 nm, c = 0.7881 nm) as shown in Figure 4(a). The matrix was found to be
Laves Phase in Alloy 718 Fusion Zone 7
http://dx.doi.org/10.5772/intechopen.70325

Figure 4. TEM bright field image with SADP pattern of (a) Laves phase in as-welded fusion zone, TEM dark field
micrograph of direct-aged fusion zone (b) γ″ precipitates with zone axis [−1 1 1].

polycrystalline in nature with face centered cubic crystal structure (a = 0.3571 nm) for the
fusion zone of higher weld cooling rates (394°C/s and above).

The aging response was also confirmed by the TEM dark field images. The respective selected
area diffraction pattern is shown in Figure 4(b). Disc-shaped γ˝ precipitates and spherical γʹ
precipitates were observed. The Laves phase morphology and its crystal structure were not
affected by the imposed thermal gradient and enhanced weld cooling rate. The script type
morphology of the Laves particles was retained for the employed weld cooling rates.

The partition ratio of the individual elements was calculated from the FE-SEM/EDS data using
dendrite microsegregation model. The partition coefficient of niobium in the FM1 fusion zone
was increased from 0.54 to 0.72 in the conventionally cooled fusion zone. This could be due to the
decrease in iron and chromium contents (Figure 3). However, the partition ratio of niobium (0.54–
0.97) in the FM2 fusion zone was found to be more than that of the FM1 fusion zone. The fusion
zones of lower weld cooling rates exhibited higher Laves phases because of the huge segregation
of niobium and molybdenum (kNb = 0.54) toward liquid. Obviously, a steep concentration gradi-
ent was built in the interdendritic liquid by the lower diffusivity and/or mobility parameter of
molybdenum through solutal undercooling. This led to a better refinement in microstructure. The
BSE micrograph of the liquid nitrogen-cooled FM2 fusion zone revealed the reduced interden-
dritic segregation as shown in Figure 5(a). The elemental mapping also confirmed the reduced
microsegregation of niobium as shown in Figure 5(b). The finer distribution of Laves particles
aided in improving the mechanical properties of the liquid nitrogen cooled weldment. However,
the characteristic temperatures in DSC analysis were not affected significantly for the liquid nitro-
gen-cooled FM1 fusion zone from that of the conventionally cooled alloy 718 fusion zone.
In the present study, liquidus temperature (primary γ) of the FM1 fusion zone was not signifi-
cantly changing from that of the base material for the lower weld cooling rates of 40–362°C/s.
But a significant increase in liquidus temperature was observed with the higher employed
cooling rates of 394 and 5107°C/s due to the enhanced molybdenum content in the matrix at
these cooling rates as shown in Figure 3. The partitioning of higher melting point solute (Mo)
to γ matrix led to the increase in the solvus temperature of γ matrix. Whereas the liquidus
8 Superalloys for Industry Applications

Figure 5. BSE image of FM2 fusion zone for a weld cooling rate of (a) 510°C/s and (b) elemental mapping in EPMA.

temperature of FM2 fusion zone was decreasing as the cooling rate was increased due to
the increased solute concentration in the matrix as per the phase diagram, at higher cooling
rates, the liquidus temperature of FM2 fusion was comparable to that of the base material.
The solidification time for each employed weld cooling rate was calculated using heat trans-
fer experiments and DSC analysis and found reduced from 2.099 to 0.12 s for the enhanced
weld cooling rate from 40 to 394°C/s. This was further reduced to 0.011 s for the liquid nitro-
gen cooling method. The SE micrographs of the fusion zones of hybrid pulsing using argon
and helium shielding gases are shown in Figure 6(a)–(f). In the present study, the modified

Figure 6. SE micrographs of (a–c) argon and (d–f) helium shielded as-welded fusion zone using hybrid pulse current.
Laves Phase in Alloy 718 Fusion Zone 9
http://dx.doi.org/10.5772/intechopen.70325

Figure 7. X-ray diffraction patterns of the fusion zone of three different weld cooling rates with FM1 in (a) as-welded
and (b) direct-aged conditions.

pulsing increased plasma momentum and electro-magnetic force inside the weld pool and led
to the refined microstructure. Thus, the interdendritic Laves phase was reduced.

The fluctuation in radiation had been reduced in the pulse frequency range of 500–2000 Hz
and therefore the heat transfer efficiency of the arc was improved. The increased plasma
momentum enhanced the arc pressure. In addition, the lower pulse ratio was resulted by the
subdivision of peak pulse time with superimposed high frequency pulsing. The combination
of the above phenomenon was giving rise to the convective flow. This aided in the equiaxed
growth ahead of columnar growth. However, the fluctuations induced by the pulsing current
alone were not aiding the fragmentation of dendrites in mushy zone. The solute enrichment
at the dendrite root caused the dendrite remelting. Hence, the finer secondary dendritic arms
were fractured and/or fragmented easily and further aided by the stirring action and/or by
viscous friction caused by the relative movement between liquid and solid metal.

The phases formed in the fusion zone were analyzed using the representative X-ray diffrac-
tograms as shown in Figure 7(a) and (b). The diffraction peaks indicated the presence of
γ matrix, MC type carbides, and Laves phase in the as-welded condition for both the FM1
and FM2 fusion zones. The lattice parameter of γ matrix was calculated using Nelson-Riley
method and found an increased lattice constant (0.36113 nm) for FM1 fusion zone due to
the increased solute (Mo) content in the dendrite. In addition, FM1 fusion zone exhibited
β-Ni4Mo phase in the as-welded condition and got dissolved after direct aging treatment as
shown in Figure 7(a) and (b). The direct-aged specimens of fusion zone showed the diffrac-
tion peaks of γ˝/γʹ precipitates, MC type carbides, and Laves phase.

4. Mechanical property characterization of weldments

The hardness distribution in the weld metal was executed through microhardness survey.
The experimental conditions are as follows:
10 Superalloys for Industry Applications

• Condition: As welded, Duration: 15 s, Load: 2.942 N.

• Condition: Direct aged, Duration: 15 s, Load: 9.807 N.

The microhardness survey on the welded samples is given in Table 2. As inferred from the
microhardness survey, the liquid nitrogen cooling method produced softer weldments than
that of the conventionally cooling method.
The increased microsegregation and the existence of Laves phases led to the increased hard-
ness in the as-welded condition for the conventionally cooled weld metal. The upper limit of
the hardness values for the as-welded and direct-aged conditions mentioned in Table 2 was
corresponding to the lower and higher weld cooling rates, respectively. Moreover, the liquid
nitrogen-cooled FM1 (solid solution filler metal) fusion zone well responded for the direct
aging process as the fusion zone hardness values were comparable with FM2 (age harden-
able filler metal) fusion zone. The results of room temperature (25°C) and high-temperature
(650°C) tensile tests conducted on the welded specimen with six levels of weld cooling rate
are given in Figure 8(a) and (b) for the conventional and liquid nitrogen cooling methods.

The room temperature tensile test data revealed that the weld strength properties in direct-
aged condition were improved with CCP technique than that of the previous works on the
same alloy system [1, 3]. The room temperature ultimate tensile strength (UTS) of the conven-
tionally cooled weldment increased with the enhanced weld cooling rate for both the FM1
(987–1105 MPa) and FM2 (1256–1284 MPa).

The UTS values of conventionally cooled FM1 fusion zone was less than that of the FM2
fusion zone after direct aging at both 25 and 650°C. However, the tensile strength of welds
was improved for the weldments cooled with liquid nitrogen. The high-temperature strength
values were increased with the enhanced weld cooling rate. The UTS of liquid nitrogen-
cooled FM1 fusion zone (1038 MPa) was higher than that of the FM2 fusion zone (1005 MPa)
for the same weld cooling rate (510°C/s). This could be due to the reduced grain growth by
the retention of molybdenum in the dendrite [11]. The microstructures were refined in FM1

Cooling method Filler metal Hardness of fusion zone (Hv)

As welded Direct aged


Conventional FM1 205–365 363–418

FM2 238–406 410–454

Liquid nitrogen cooling FM1 221–269 310–475

FM2 204–237 309–475

Hybrid pulsing FM1-Argon 250–375 350–415

FM1-Helium 260–380 375–418

FM2-Argon 230–250 330–440

FM2-Helium 210–280 350–438

Table 2. Hardness of fusion zone.


Laves Phase in Alloy 718 Fusion Zone 11
http://dx.doi.org/10.5772/intechopen.70325

Figure 8. Tensile properties [(a, b) tensile strength and (c) strain] of conventionally and cryogenically cooled FM1 and
FM2 weldments at 25 and 650°C.

fusion zone due to the addition of molybdenum which promoted solutal undercooling by
the concentration gradient. Hence, the combined effect of thermal and solutal undercooling
resulted in a refined microstructure.
The fracture surfaces of the room temperature tensile specimens at 25°C for DA conditions
revealed the equiaxed dimple morphology. The fracture surface investigation in SEM indi-
cated a detrimental nature of the Laves phase in fracture process even at 650°C. The fracto-
graphs of 650°C tensile tested specimen of FM1 and FM2 are as shown in Figure 9(a) and (b)
for the conventional cooling process.
Among the six fusion zones of different weld cooling rates, the FM1 fusion zone exhibited
deep dimple features at 650°C. The fractured surfaces of 650°C testing exhibited a mixed
mode (inter and transgranular modes) of fracture with a unique dendritic pattern. The frac-
ture was progressed along the Laves phase. The Laves particles were observed inside the
dimple surface for the fusion zones of 40°C/s as shown in Figure 9(b). The microcracks were
initiated preferentially by decohesion of laves phase–γ matrix interface under the action of
a tensile stress and resulted in a premature failure. The wedge type cracking features were
observed in both FM1 and FM2 fusion zones.
12 Superalloys for Industry Applications

Figure 9. Fractographs of (a, b) conventionally cooled and (c) liquid nitrogen-cooled fusion zones tensile tested at 650°C.

The fractographs of the liquid nitrogen-cooled weldments exhibited transgranular frac-


ture as shown in Figure 9(c). It was proved that the tensile properties of the alloy 718
weldment were reduced at room temperature conditions, especially the weld ductility.
Similar results were obtained at room temperature in the present study. In addition, it
was observed in the present work that at 650°C tensile properties were also reduced as
the Laves particles favored crack initiation and continuous Laves network aided the crack
propagation. This led to the easier fracture process. The fracture process was progressed
by the nucleation of voids and subsequent growth of macroscopic cracks along the weaker
laves-matrix interface even at 650°C. Thus, weld ductility was reduced. As the Laves net-
work was disrupted and refined, equiaxed dendritic microstructure associated with fine
and discrete Laves particles enhanced the tensile properties both at 25 and 650°C. The
plastic strain of the cryogenically cooled weld metal was higher than that of the conven-
tionally cooled weld metal as shown in Figure 8(c). The liquid nitrogen-cooled fusion zone
had increased molybdenum content in the dendrite (4–5 wt%) and molybdenum-bearing
phase was observed in the XRD analysis of FM1 fusion zone as shown in Figure 7(a). These
phases pinned the grain boundaries and enhanced the plastic strain in liquid nitrogen-
cooled weldments.
The room temperature mechanical properties of the hybrid pulsing weldments were evalu-
ated and the maximum tensile strength of 1155 and 1100 MPa for argon and helium shielded
FM1 fusion zones at 500 and 2000 Hz, respectively. Similarly, maximum tensile strengths were
obtained at 2000 Hz in the argon and helium shielded FM2 (1330 MPa) fusion zones. The maxi-
mum yield strength (965 MPa) was obtained in the intermediate pulse frequency (1250 Hz) for
the argon shielded FM1 fusion zone and (856 MPa) at 2000 Hz in the helium shielded fusion
zone. FM2 fusion zone exhibited a maximum of 1138 MPa yield strength for both argon and
helium shielded fusion zone at 1500 and 2000 Hz, respectively. The maximum weld ductil-
ity was demonstrated for the helium shielded FM1 weldments than that of the other hybrid
pulsing weldments. The high-temperature tensile testing of the transverse welded specimens
revealed an ultimate tensile strength values ranging from 989.53 to 1030.15 MPa (±16.79 MPa)
and 0.2% yield strength values from a minimum of 843.33 MPa to a maximum of 885 MPa
(±17.68 MPa). The ductility of the weld was lower in the range of 3.48–3.6% (±0.14) and a plastic
strain of 1–1.26% (±0.05%).
Laves Phase in Alloy 718 Fusion Zone 13
http://dx.doi.org/10.5772/intechopen.70325

5. Inferences

The interdendritic Laves phase formation during GTA welding of alloy 718 has been inves-
tigated using enhanced weld cooling rates and change of weld metal chemistry. The volume
fraction of Laves phase was reduced from 45.95 to 8% with the enhanced weld cooling rate by
the combination of modified pulse current and helium shielding gas for both FM1 and FM2
fusion zones. This was further reduced to 0.1% while employing cryogenic cooling during
GTA welding process. The high energy density processes minimized Laves phase and prone
for HAZ microfissures. GTA welding process employed with liquid nitrogen cooling aided in
minimizing laves phase and free of HAZ microfissures. Enhanced weld efficiency on UTS and
0.2% YS at 25°C was observed to the tune of 85–93% by employing cryogenic cooling in GTA
welding process. Similar improvement in weld efficiency at 650°C was observed. However,
the evaluated weld efficiencies with cryogenically cooled weld metal were marginally lower
than the previous works in EB and LB welds only by 2–3%. Moreover, it was observed that
the Laves network influenced the strength of the weldment at 650°C. The modification of weld
metal chemistry with Mo solute element through solid solution filler metal (FM1) promoted
solutal undercooling, in addition to the thermal undercooling. Thus, the microstructures were
refined and Laves phase formation was reduced. The intermediate pulse frequencies were
aiding better Laves phase control for the argon shielded GTA welding process and the same
results were obtained with 2000 Hz pulse frequency in the helium shielded process. This could
be due to the combined effect of longitudinal temperature gradient while using different
shielding gases and shape factor of the pulse wave form.

Author details

S.G.K. Manikandan1*, D. Sivakumar1 and M. Kamaraj2

*Address all correspondence to: nehakutty06@gmail.com

1 Indian Space Research Organisation, India

2 Indian Institute of Technology Madras, India

References

[1] Mills WJ. Effect of microstructural variations on the tensile and fracture toughness prop-
erties of Inconel 718 weldments. In: Loria PA, editor. Proc. Conf. on 718 alloy. PA: TMS;
1984. pp. 845-858

[2] Reddy GM, Murthy CVS, Srinivasa Rao K, Prasad RK. Mint: Improvement of mechani-
cal properties of Inconel 718 electron beam welds—influence of welding techniquesand
postweld heat treatment. International Journal of Advanced Manufacturing Technology.
2009;43:671-680
14 Superalloys for Industry Applications

[3] Ram GDJ. Effect of Laves phase on mechanical properties on Inconel 718 welds [Thesis].
Chennai: IIT Madras, Department of Metallurgical and Materials Engineering; 2004

[4] Sivaprasad K, Ganesh Sundararaman S. Mint: Influence of weld cooling rate on micro-
structure and mechanical properties of alloy 718 weldments. Metallurgical and Materials
Transactions A. 2008;39(9):2115-2127

[5] Zhang W, Liu L. Mint: Solidification microstructure of directionally solidified superalloy


under high thermal gradient. Rare Metals. 2012;31(6):541-546

[6] Wang J, Kusumoto K, Nezu K. Mint: Analysis of electrical characteristics for hybrid
pulsed micro-tungsten inert gas welding arc. Science and Technology of Welding and
Joining. 2004;9(4):369-373

[7] Amuda MOH, Mridha S. Mint: Grain refinement and hardness distribution in cryogeni-
cally cooled ferritic stainless steel welds. Materials Design. 2013;47:365-371

[8] Banovic SW, Du Pont JN, Marder AR. Mint: Dilution and microsegregation in dissimilar
metal welds between super austenitic stainless steel and nickel base alloys. Science and
Technology of Welding and Joining. 2002;7(6):374-383

[9] Knorovsky GA, Cieslak MJ, Headley TJ, Romig Jr. AD, Hammetter WF. Mint: Inconel
718: A solidification diagram. Metallurgical and Materials Transactions A. 1989;
20(10):2149-2158

[10] Du Pont JN, Robino CV, Micheal JR, Notis MR, Marder AR. Mint: Solidification of
Nb-bearing superalloys: Part I. Reaction sequences. Metallurgical and Materials
Transactions A. 1998;29A:2785-2796

[11] Han D, Liu F, Jia D, Qi F, Yang H, Sun W, Hu Z. Effect of Mo addition on the grain
growth of IN718 alloy. Materials Science Forum. 2015;816:594-600
DOI: 10.5772/intechopen.70256

Chapter 2
Provisional chapter

High-Temperature Oxidation
High-Temperature Oxidation of
of Superalloy
Superalloy C-263
C-263of
of
Rings for
Rings for Aircraft
Aircraft Engines
Engines

Citlalli Gaona Tiburcio, Alejandro Lira Martinez,


Citlalli Gaona Tiburcio, Alejandro Lira Martinez,
Jorge
Jorge Taboada Solis, Patricia
Taboada Solis, Patricia Zambrano
Zambrano Robledo,
Robledo,
Francisco Estupiñán López,
Francisco Estupiñán López, Jose Cabral Miramontes
Jose Cabral Miramontes
and Facunda and
Almeraya Calderón
Facunda Almeraya Calderón
Additional information is available at the end of the chapter

Additional information is available at the end of the chapter

http://dx.doi.org/10.5772/intechopen.70256

Abstract
The present investigation was conducted to study the oxidation kinetics of nickel-based
superalloy 263, used in the manufacture of rings for aircraft engines. For carrying out
this study, we first conducted microstructural characterization of the pieces using the
techniques of optical microscopy, scanning electronic microscopy, and X-ray diffraction.
Subsequently, using the thermogravimetric analysis, the kinetic oxidation of the metal
was performed in a temperature range between 700 and 1000°C, using atmospheres of
O2. The results of the micrographs show the formation of a protective oxide film on the
surface of the material in different oxidizing agents. Finally, it was found that the kinet-
ics of high-temperature oxidation of the superalloy C-263 obeys the parabolic rate law.

Keywords: superalloys, oxidation, thermogravimetric, aircraft engines

1. Introduction

In order to meet the current demand for the aerospace industry, the production of advanced
materials is required that ensure the design and manufacture of a robust product and that
meet customer expectations, increased engine performance for fuel efficiency, mechanical
strength of the components, and at the same time be lighter and less expensive. Therefore,
there is a great interest in the development and study of superalloys that will generate

© 2018 The Author(s). Licensee IntechOpen. This chapter is distributed under the terms of the Creative
Commons Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use,
distribution, and reproduction in any medium, provided the original work is properly cited.
© 2016 The Author(s). Licensee InTech. This chapter is distributed under the terms of the Creative Commons
Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use, distribution,
and reproduction in any medium, provided the original work is properly cited.
16 Superalloys for Industry Applications

mechanically resistant aircraft, capable of withstanding corrosive environments at high tem-


peratures. Inside a combustion chamber at duty, on a gas turbine engine of aircraft, very
aggressive corrosive agents exist. One of these is sulfur, which can deteriorate the materials
and reduce their useful life [1].
Nickel-based superalloys are generally used at temperatures above 540°C in very aggres-
sive environments. Seamless rolled rings are made of superalloy Haynes C-230 or C-263 and
used in the combustion chamber of gas turbine engines, which are exposed to corrosive gas
mixtures. One of those gases is SO2. However, because of its machining process, its corrosion-
resistant properties may be compromised [2, 3].
Sulfur is generally present as an impurity in fuels and air. When combustion takes place with
excess of air to ensure complete combustion of fuel, sulfur reacts with oxygen to form mainly
SO2, which is a corrosive gas. However, sulfidation in oxidizing environments is frequently
accelerated by other impurities such as sodium, potassium, and chlorine, making possible the
so-called hot corrosion mechanism [4].

Superalloys exposed in SO2 environments generally form oxides and/or sulfides as corro-
sion products, which depend strongly on temperature. The highest corrosion rate is normally
related to the formation of sulfides [1]. Sulfides provide paths for rapid outward diffusion of
metals resulting in rapid corrosion attack. For nickel, the corrosion rate in this environment is
around 600°C, and above 800°C, the rate decreases with increasing temperature.
Haynes 263 is a nickel-chromium-tungsten-molybdenum alloy that combines high-temper-
ature strength, resistance to oxidizing environments up to 1149°C for prolonged exposures,
premier resistance to nitriding environments, and excellent long-term thermal stability [5].

The manufacturing process for forging rings [6] of superalloys may be used in turboreactors
or components of the high-temperature section of a gas turbine such as the combustion cham-
bers of the intermediate-temperature section (Figure 1) [7].

Figure 1. Seamless rolled rings for aircraft engines [6].


High-Temperature Oxidation of Superalloy C-263 of Rings for Aircraft Engines 17
http://dx.doi.org/10.5772/intechopen.70256

There are a large number of nickel-based superalloys in the world such as the C-263 which
contains multiple phases, depending on the alloying elements. The most prevalent phase in
this superalloy is the gamma (γ) phase, with a cubic crystalline structure centered on the
faces. Ni-based superalloys are hardened, due to the formation of solid solutions, using a
variety of substitution alloying elements in the γ-structure such as molybdenum. In the case
of superalloy C-263, aluminum and titanium only make up about 3% of the total composition.
However, these components are important for the properties of the materials associated with
superalloys, due to the formation of the γʹ-phase [8].

In metallic corrosion, the oxidation of alloys at high temperatures can be treated as a special
case, which considers the material destruction due to chemical causes, in which solid phases
interact either with a liquid agent or a gaseous agent. The latter case involves reducing and
oxidizing gases, steam, and even free oxygen. The oxidation is determined by the internal
mobility of the solid phases and mainly diffusion in solid state. It is well known that alloying
with chromium improves the oxidation resistance of iron at high temperatures [9].

The principal objective in this research was to study the oxidation kinetics of nickel-based
superalloy C-263 in a temperature range of 700–1000°C using atmospheres of O2 for 48 h.

2. Experimental procedure

The material used in this research was Haynes C-263 superalloy. The specimens were sections
of 4 × 4 × 2.5 mm. The surface of samples was ground using 2000 grade grit paper, rinsed with
distilled water, and degreased with acetone [10].

Figure 2. Thermogravimetric analyzer TA Instruments.


18 Superalloys for Industry Applications

The oxidation test was performed in a thermogravimetric analyzer TA Instruments Hi Res


TGA 2950 (Figure 2), for 48 h. Experiments were conducted in gaseous atmosphere of O2–N2
with a flow of 75 ml/min at an interval of temperatures of 700–1100°C (+2°C). For each speci-
men a weight gain measurement in an electronic microbalance (sensitivity 10−6 g) was set.

The oxidized samples were analyzed in a scanning electron microscopy (SEM; FEI Nova
NanoSEM 200) coupled with an energy-dispersive X-ray spectroscopy (EDS) system, in order
to understand the oxidation phenomena in terms of scale morphology and oxidation product
distribution.

3. Results and discussion

3.1. Chemical analyzer

The chemical composition of superalloy C-263, used in the present study, is given in Table 1.
The chemical analysis was performed using the technique of X-ray fluorescence.

3.2. Alloy microstructure

The microstructure of the alloys in the study (Figure 3) is composed of an austenitic matrix
gamma (γ) and twins that are typical in this material, with intermetallic precipitates of
gamma prima (γʹ). The precipitates in the microstructure are in the form of carbides and some
borides, and the grains are regular.

3.3. Thermogravimetric analyzer

The kinetic measurements indicated that, in general, the alloys presented a parabolic behav-
ior, according to

(∆ m/A) 2 = K (t - t ) (1)


p o

where (∆m/A) is the weight gain per unit area; t and to are the final and initial time, respec-
tively; and Kp is the parabolic rate constant [11].

The increase in mass gain, higher as temperature increases, is significantly lower as the expo-
sure time increases. This progressive decrease in the rate of oxidation indicates the formation
of a compact and well-adhered oxide. According to Wagner’s [12] theory, systems subjected
to high temperature and controlled by diffusion processes, through the network of the oxide
layer, follow an oxidation kinetics described by a parabolic-type equation.

Chemical composition (% wt.)


Material Ni Cr Co Mo Ti Fe Al Mn Si Cu C

C-263 51.80 20.20 19.90 6.00 2.30 0.69 0.60 0.62 0.40 0.19 0.05

Table 1. Chemical composition of superalloy C-263.


High-Temperature Oxidation of Superalloy C-263 of Rings for Aircraft Engines 19
http://dx.doi.org/10.5772/intechopen.70256

Figure 3. Microstructure of superalloy C-263.

Figure 4. Dependence of the weight gain on the oxidation time in O2 at (a) 700°C, (b) 800°C, (c) 900°C, and (d) 1000°C
for 48 h.
20 Superalloys for Industry Applications

Oxidation kinetics of superalloy C-263 was studied at 700, 800, 900, and 1000°C; Figure 4
shows the weight change per unit area versus time. Evidently, the oxidation rate increases as
the temperature rises. A parabolic behavior was found at all testing temperatures. The kinetic
results are in agreement with those reported in the literature in the sense that the kinetic
behavior is parabolic [13, 14].

In order to better visualize this behavior, the square of the mass increase per unit area for
superalloy C-263 at the temperatures mentioned above has been plotted in Figure 5. For all
the cases studied, there is a linear relationship between both variables. This fact confirms
that the oxidation of superalloy at the four test temperatures follows a parabolic law. The
indicated graphs also allow to calculate the parabolic oxidation rate constants (see Table 2).
Knowing the parabolic rate constant for each temperature, the activation energy of the oxida-
tion reaction can be calculated from the Arrhenius equation, which relates Kp to the tempera-
ture by the expression:

Kp= Ko e (−RT)
Q
___
(2)

Figure 5. Parabolic oxidation of superalloy C-263.


High-Temperature Oxidation of Superalloy C-263 of Rings for Aircraft Engines 21
http://dx.doi.org/10.5772/intechopen.70256

Temperature (°C) Parabolic oxidation rate constants (mg2/cm4 h)


700 4.18 × 10−8

800 7.21 × 10−8

900 7.66 × 10−6

1000 7.16 × 10−5

Table 2. Values of the parabolic oxidation rate constant (mg2/cm4 h).

where Q is the activation energy; R is the gas constant, in joules or calories; Ko is the rate con-
stant at room temperature; and T is the absolute temperature.
In Figure 6 the parabolic oxidation rate constant is obtained against the inverse of the tem-
perature. The value of the activation energy Q is 28.37 kcal/mol and is indicative that the
oxidation process is diffusion controlled through the layer of oxides formed.
The oxide layer in the superalloy samples at 700, 800, and 1000°C remained adherent to the
substrate, but not at 900°C, which, after finishing the test, was probably due to the stresses
generated with the thermal contraction.
Garcia-Alonso et al. studied the oxidation kinetics of the MA 956 superalloy in the temperature
range of 800–1200°C for up to 200 h exposure. During oxidation the alloy develops a fine, com-
pact, and very well-adhered alpha-alumina layer, the thickness of which increases with increasing

Figure 6. Constant of the oxidation rate of superalloy C-263 as a function of temperature.


22 Superalloys for Industry Applications

time and temperature. The oxidation kinetics obeys a subparabolic-type behavior, and the oxida-
tion process would be controlled by alpha-alumina and below 900°C by 7-alumina.
Other authors have studied the behavior of high-temperature oxidation of nickel-based super-
alloys in different temperature ranges, where the kinetics of oxidation obeys the parabolic law
by the addition of elements such as aluminum, titanium, niobium, or yttrium [15, 16].
The Encinas-Oropesa study targeted at characterizing the oxidation behavior of a new nickel-
based disk alloy (RR1000) at intermediate temperatures (700–800°C for exposures up to 200 h).
The mass gain data obtained have been used to derive oxidation reaction rate parameters, using
established methodologies, with parabolic rate constants varying between 1.4 × 10−5 mg2/cm4/h
at 700°C and 8.4 × 10−4 mg2/cm4/h at 800°C [17].

3.4. Scanning electron microscopy (SEM)

The results obtained by SEM on the oxidized specimens revealed different morphologies
depending upon the temperature of testing.

Figure 7. Superalloy C-263 at 700°C for 48 h, superficial morphology, cross section, and X-ray map for O, Ni, Co, and Cr.
High-Temperature Oxidation of Superalloy C-263 of Rings for Aircraft Engines 23
http://dx.doi.org/10.5772/intechopen.70256

Figure 8. Superalloy C-263 at 800°C for 48 h, superficial morphology, cross section, and X-ray map for O, Ni, Ti, and Cr.

The superficial morphology at 700°C presents fine-grained oxides and brittle banded agglom-
erates (Figure 7). Cross-sectional analysis of the samples by SEM/EDS on the layer formed on
all alloys suggested the formation of titanium- and chromium-rich oxides.
At 800°C morphology with banded agglomerates, rich in chromium and titanium, is observed;
these same elements develop a thin and not very homogeneous layer of chromium oxide and
titanium (see X-ray map; Figure 8).

Observing the morphology obtained from the superalloy C-263 heat treated at 900°C for
48 h (1000 X), a surface totally covered by a great amount of particles with different sizes
and defined morphologies can be noted, although they are more evident those that have
form of bars, with larger particle size. Figure 9 shows the formation of an abundant oxide
24 Superalloys for Industry Applications

Figure 9. Superalloy C-263 at 900°C for 48 h, superficial morphology, cross section, and X-ray map for O, Ni, Co, Ti,
and Cr.

layer, in which two layers of oxide, internal and external, can be observed. The inner layer
consists mainly of chromium oxide, and the outer layer is formed by an oxide of cobalt and
nickel. Between both layers there is an oxide of titanium.

The presence of chromium in this type of superalloys not only improves the mechanical prop-
erties by hardening at high temperatures but also stabilizes the phase. Oxidation studies in
superalloys with the presence of aluminum and chromium have shown a high tendency of
formation of continuous and protective films above 900°C [18–20].

When this superalloy C-263 was treated at 1000°C for 48 h, different morphologies and par-
ticle sizes are observed. On the one hand, defined grains with particle sizes between 5 and
10 μm and in some areas the formation of smaller particle agglomerates covering the grains
High-Temperature Oxidation of Superalloy C-263 of Rings for Aircraft Engines 25
http://dx.doi.org/10.5772/intechopen.70256

Figure 10. Superalloy C-263 at 1000°C for 48 h, superficial morphology, cross section, and X-ray map for O, Ni, Co, Ti,
and Cr.

are observed. In X-ray map can be observed, the formation of an abundant oxide layer, in
which two layers of oxide, internal and external, is observed; the inner layer is made up
mostly of chromium oxide, and the outer layer is formed by a cobalt and nickel oxide (see
Figure 10; 1000 X).

By SEM-EDS at 800, 900, and 1000°C, the formation of a larger amount of Cr oxide, Ti, and Ni
on the surface of superalloy was observed. It was determined that while the temperature of
the thermal treatment increased, the amount of the oxide is increased.

The growth rate of Cr2O3 scales at high temperatures is greatly reduced by the presence of
elements as nickel, titanium, and cobalt [21].
26 Superalloys for Industry Applications

4. Conclusions

• The kinetics of high-temperature oxidation of the superalloy C-263 obeys the parabolic rate
law for temperatures 700, 800, and 1000°C.

• Cross-sectional analysis, by SEM/EDS, of the layer formed on all samples suggested the
formation of titanium- and chromium-rich oxides and in some cases cobalt and nickel
oxide after 900°C.

• The present investigation found that at 700°C, there is almost no oxide on the surface of the
superalloy, only seen a little agglomerates of Mn, Cr, and Ni as major components of the
superalloy matrix.

Author details

Citlalli Gaona Tiburcio1, Alejandro Lira Martinez2, Jorge Taboada Solis1,


Patricia Zambrano Robledo1, Francisco Estupiñán López1, Jose Cabral Miramontes1
and Facunda Almeraya Calderón1*

*Address all correspondence to: falmeraya.uanl.ciiia@gmail.com

1 Universidad Autónoma de Nuevo León (UANL), Facultad de Ingeniería Mecánica


y Eléctrica (FIME), Centro de Investigación e Innovación en Ingeniería Aeronáutica
(CIIIA), Av. Universidad s/n. Ciudad Universitaria. San Nicolás de los Garza,
Nuevo León, México

2 Universidad Autónoma de Ciudad Juárez, Instituto de Ingeniería y Tecnología, Cd Juárez,


Chihuahua, México

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pdf

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[7] Pollock T, Tin S. Nickel-based superalloys for advanced turbine engines: Chemistry,
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[8] Pettit F, Meier G. Oxidation and hot corrosion of superalloys. TMS. 1984;1:651-687

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[10] ASTM E3-11. Standard Guide for Preparation of Metallographic Specimens. 100
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[12] Wagner C. Atom Movements. ASM; 1951. p. 153

[13] Nakamura Y. Metallurgical Transactions. 1974;5:909

[14] Golightly FA, Wood GC, Stott FH. Oxidation Metals. 1980;14(3):217

[15] Weng F, Yu H, Chen C. Corrosion Science. 2013;75:58-66

[16] Taylor MP, Evans HE, Stekovic S. Surface and Interface Analysis. 2015;47(3):362-370

[17] Encinas OA, Simms NJ, Nicholls JR, Hardy MC. Journal Materials at High Temperature.
2009;26(3):241-249

[18] Reed RC. The Superalloys Fundamentals and Applications. 1st ed. UK: Cambridge
University Press; 2006. p. 390

[19] Moussa SO, Morsi K. Journal of Alloys and Compounds. 2006;426(1-2):136-143

[20] Szacalos P, Lundberg M, Pettersson R. Corrosion Science. 2006;48(7):1679-1695

[21] Martínez-Villafañe A, Chacón NJ, Gaona TC, Almeraya CF, et al. Materials Science
Engineering A. 2003;A263:15-19
DOI: 10.5772/intechopen.76083

Provisional chapter
Chapter 3

Hot
Hot Corrosion
Corrosion of
of Superalloys
Superalloys in
in Boilers
Boilers for
for Ultra-
Ultra-
Supercritical
Supercritical Power
Power Plants
Plants

Nageswara Rao Muktinutalapati,


Nageswara Rao Muktinutalapati,
Arivazhagan Natarajan and Moganraj Arivarasu
Arivazhagan Natarajan Moganraj Arivarasu

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Additional information is available
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http://dx.doi.org/10.5772/intechopen.76083

Abstract

The coal-based power plants have been plagued by twin problems—low thermal effi-
ciency and emission of high level of pollutants into the environment. Over the last few
decades, attention was paid by researchers worldwide to overcome these problems and to
design, build, and operate coal-based plants with improving efficiency levels and reduc-
ing emission levels. Operating the power plants with higher levels of steam temperature
and pressure was adopted as the direction toward achieving the needed improvements.
The requirement to operate the plants with increasingly higher levels of temperature and
pressure made it necessary to design the components with superalloys. Hot corrosion
then becomes a major design consideration, particularly for superheaters and reheaters.
Thus, it becomes important to study the hot corrosion behavior of candidate superal-
loys. The present chapter attempts to review the work done over the last two decades
to understand the hot corrosion behavior of superalloys in the context of their use in
advanced coal-based power plants.

Keywords: ultra-supercritical coal fired power plants, nickel-based superalloys, hot


corrosion, fireside corrosion, sulfidation

1. Introduction

Ultra-supercritical (USC) power plants are expected to overcome two challenges—(i) an


increase in demand for electricity and (ii) a significant reduction in the enhanced greenhouse
effect due to CO2 emission from the fossil fuel. By increasing the operating temperature and
pressure of the steam systems, an increase in the power plant efficiency and a major reduction

© 2016 The Author(s). Licensee InTech. This chapter is distributed under the terms of the Creative Commons
© 2018 The Author(s). Licensee IntechOpen. This chapter is distributed under the terms of the Creative
Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use,
Commons Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use,
distribution, and reproduction in any medium, provided the original work is properly cited.
distribution, and reproduction in any medium, provided the original work is properly cited.
30 Superalloys for Industry Applications

in the CO2 emission from the power plants based on firing pulverized coal can be realized [1].
The goal of the latest designs in power plants is to generate 760°C steam. In the process, metal
surface temperature of the key components such as superheaters and reheaters may reach as
high temperature as 800°C [2]. The materials used for superheaters and reheaters in coal-fired
boiler environments always suffer coal ash hot corrosion at elevated temperatures [3, 4]. Coal
ash hot corrosion is the result of competition between oxidation and sulfidation. Sulfidation
comes into picture as the materials get exposed to high-temperature combustion gases con-
taining sulfate coal ash [5]. Superalloys, in particular, nickel-base superalloys, have been the
candidate materials for application in boilers for ultra-supercritical power plants based on
firing coal. Compared to different types of high-temperature steels, nickel-based superalloys
are well known for their superior resistance to coal ash hot corrosion [6, 7]. While there have
been several publications on use of high-temperature materials in advanced power plants, a
systematic review of application of superalloys for critical components facing hot corrosion
and high temperature creep loading conditions in advanced coal-based power plants has not
been carried out in the recent years. This chapter proposes to bridge this gap.

2. What are ultra-supercritical power plants?

Because of the abundant availability of coal reserves in the world, the use of coal for electricity
generation has been done extensively. Coal has thus dominated as fuel for electricity genera-
tion, even though many modern technologies have emerged for power generation. Use of coal
for power production is, however, beset with serious problems. Coal-based power plants emit
pollutants and CO2 at high levels. Further, the efficiency of the conventional coal-based power
plants has been very low, 35–40%. The efficiency of the power plant can be increased by increas-
ing the operating steam temperature and pressure. Development studies were undertaken
worldwide to build power plants with increased values of these two operating parameters. In
addition to increased thermal efficiency, an increase in these two parameters would lead to a
reduction in greenhouse gases, an issue where the public is becoming increasingly conscious of.
Several of the existing coal-based power plants belong to the category of subcritical power
plants operating at a steam pressure of ~22 MPa and a steam temperature of ~550°C; the ther-
mal efficiency of these plants is in the range of 35–37%. The plants operating in the tempera-
ture range of 540–580°C with steam pressure extending up to 25 MPa are termed supercritical
power plants; their efficiency is of the order of 45%. Ultra-supercritical power plants operate

Main steam Main steam Reheat steam Average CO2 emissions


pressure, MPa temperature, °C temperature, °C efficiency (g/KWh)
Subcritical <22.1 Up to 565 Up to 565 36 766–789

Supercritical 22.1–25 540–580 540–580 45 722

Ultra-supercritical >25 >580 >580 >45 <722

Table 1. Classification of power plant conditions [8].


Hot Corrosion of Superalloys in Boilers for Ultra-Supercritical Power Plants 31
http://dx.doi.org/10.5772/intechopen.76083

at temperature higher than 580°C and pressure higher than 25 MPa, leading to an efficiency
level of more than 45%. All over the world, several plants have been set up conforming to
ultra-supercritical technology. Recent advances in the alloy making and processing capability
to produce different items of hardware from these alloys have resulted in the possibility of
setting up advanced ultra-supercritical power plants, where the operating temperature would
be 700°C or more and operating pressure in the range of 30–35 MPa. The associated efficiency
is expected to be equal to or better than 50%. These advancements in terms of temperature
and pressure parallelly result in a reduction in emitted CO2 levels. Table 1 gives the details.

3. Hot corrosion in coal-fired boilers

Materials that exhibited strength to withstand the higher temperatures and pressures present
in the superheaters of supercritical and ultra-supercritical advanced boilers with required
stress rupture strength were available, but they proved to be especially susceptible to corro-
sion by certain coals, most notably high sulfur-bearing varieties.
The cause of this type of corrosion, referred to as coal ash corrosion or hot corrosion or fire-
side corrosion in advanced power plant terminology was soon understood. It is now gener-
ally accepted to be due to the presence of liquid alkali iron trisulfates on the surface of the
superheater and reheater tubes beneath an overlying ash deposit. Coal ash corrosion or hot
corrosion is a widespread problem for superheater and reheater tubes, especially when high
sulfur, high alkali, and high chlorine coals are used, and is a crucial problem that needs to be
resolved before advanced ultra-supercritical boilers can be deployed. The loss from corrosion
increased with high levels of SO2, alkali sulfates, and temperature.

Performance of nickel superalloys in such industries as aerospace or gas or marine turbines


has been well documented. However, it is important to note that the operating conditions
within a coal-fired boiler are very different in terms of the service environment. Hot corrosion
as it occurs in coal-fired boilers is a complex topic since it is a consequence of the combined
effect of combustion gas atmosphere, fly ash deposits, and the alloy itself.

4. Components/subsystems subjected to hot corrosion in ultra-


supercritical power plants

High-performance materials are required to be used for the manufacture of different sections
in boilers and steam turbines of an ultra-supercritical power plant. Table 2 summarizes the
prime design requirements for the selection of materials for various critical parts in boilers
and steam turbines. The superheater and reheater tubing are among the sections exposed to
severe environmental conditions. The outside surface of the tubing suffers fireside coal ash
corrosion, while the internal surface faces steam-side oxidation conditions. In addition, the
materials used for the subject tubing have to possess adequate stress rupture strength, as they
are subjected to long hours of mechanical loading at elevated temperatures.
32 Superalloys for Industry Applications

Design requirements
Boiler

 Headers/steam pipes Thermal fatigue strength, weld strength

 Reheater and superheater tubes Creep rupture strength and fireside corrosion resistance

Steam turbine

 Casings/shells Steam-side oxidation resistance

 Bolting Resistance to stress relaxation up to maximum steam temperature

 Rotors/discs Steam-side oxidation resistance, creep rupture strength, resistance to thermal


fatigue cracking

 Vanes/blades Steam-side oxidation resistance, solid particle erosion resistance

Table 2. Components in ultra-supercritical power plants where superalloy grades have come into consideration.

5. When does the designer choose superalloys for these components?

Development of USC power plants requires high-performance alloys able to resist the high
temperature and pressure conditions occurring in such plants. Materials for superheaters and
reheaters need to possess high creep strength and fireside corrosion resistance when it comes
to fulfilling the requirements of highly efficient power plants. Development of qualified alloys
for boiler heat exchangers was a very important task in the last decade. At temperatures higher
than about 600°C, martensitic alloys are limited by their creep strength performance [25].
Accordingly, substitution of ferritic and martensitic materials with more creep-resistant mate-
rials became necessary. Aiming at efficiencies above 40%, iron-base austenitic alloys came for
consideration and design with nickel-base superalloys became essential for 700°C technology.
Since the beginning of advanced ultra-supercritical power plant concept in the 1990s in
Europe, different nickel-based superalloys have been evaluated for their fireside corrosion,
steam-side oxidation, and resistance to creep and stress rupture. Table 3 gives the chemical
composition of nickel-based superalloys that have been the subject of studies in the context of
their usage on USC power plants.

6. Overview of work done in the area by different researchers

A number of superalloy grades were studied by different researchers for their hot corrosion
behavior in USC power plants. Table 4 gives a summary of these studies. Different material
characterization techniques were adopted to study the nature of corrosion products appear-
ing on the exposed surface; Table 5 gives a list of them. Based on the characterization, conclu-
sions were drawn on the phases occurring in the scale resulting from hot corrosion. Table 6
summarizes the findings of different authors for the two superalloy grades 617 and 740. Some
of the studies carried out in the past also looked into the relative performance of different
superalloy grades in USC power plant environments. Published information in this respect
has been summarized in Table 7.
Sl. No. Material Ni Cr Co Mo W Al C Fe Mn Si S Ti Cu B Nb La P Refs.
1 Inconel 740 49.5 25.0 20 0.5 — 0.9 0.03 0.7 0.3 0.50 <0.002 1.8 <0.1 0.002 2.0 — <0.002 [9]

2 Inconel 740H 49.0 25.0 20 0.5 — 1.35 0.03 0.7 0.3 0.15 <0.002 1.35 <0.1 0.002 1.5 — <0.002 [10]

3 Inconel 617 >44.5 20.0–24.0 10.0–15.0 8.0–10.0 — 0.8–1.5 0.05–0.15 <3.0 <1.0 <1.0 <0.015 <0.6 <0.5 <0.006 — — — [11]

4 Haynes 230 57 22 <5.0 2.0 14 0.3 0.1 <3.0 0.5 0.4 — <0.1 — — <0.5 — — [12]

5 Haynes 282 57 20 10 8.5 — 1.5 0.06 <1.5 <0.03 <0.15 — 2.1 — 0.005 — — — [13]

6 Alloy 263 Bal. 19.0–21.0 19.2–21.0 5.6–6.1 — 1.9–2.4 0.04–0.08 <0.7 <0.60 <0.40 <0.007 2.4–2.8 <0.20 <0.005 — — — [14]

Table 3. Chemical compositions of candidate superalloy grades for ultra-supercritical power plant applications.
http://dx.doi.org/10.5772/intechopen.76083
Hot Corrosion of Superalloys in Boilers for Ultra-Supercritical Power Plants
33
34 Superalloys for Industry Applications

Sl. No. Super alloy Refs.


1 740 [5, 15–19]

2 740H [17, 20]

3 Haynes 282 [21]

4 Alloy 263 [17, 18]

5 Alloy 617 and derivatives [17, 18, 20, 22, 23]

6 600,601,690,602CA,214,45TM,HR160,693 [24]

7 Alloy 230 [20, 24]

Table 4. Superalloy grades studied for their hot corrosion behavior in USC power plat environments.

Sl. No. Characterization techniques used


1 Thermogravimetric analysis (TGA)

2 Scanning electron microscopy (SEM)

3 Energy-dispersive spectroscopy (EDS)

4 X-ray diffraction (XRD)

5 Electron-probe microanalysis (EPMA)

Table 5. Techniques used by researchers to characterize the hot corrosion in simulated USC power plants.

Sl. No. Material Phases Refs.


1 Alloy 740 NiO, Cr2O3, CrS, Ni3S2, (Ni, Co)Cr2O4, Fe(CrAl)2O4 [15]

3 Alloy 740 Co3S4, Ni3S2, (Ni, Co)Cr2O4, Al2O3, TiO2, NaKS2O7, Cr2O3, [19]

2 Alloy 740 Cr2(SO4)3, Ni3S2, Co3S4, CrS, TiS, [5]

4 Alloy 617 Cr2O3, Al2O3, TiO2, CrS,NiCr2O4, CoCr2O4, FeCr2O4, Fe2O3, Cr2(SO4)3, NiO [23]

Table 6. Phases observed in the scale formed after hot corrosion of different superalloy grades in simulated USC power
plant environment.

Sl. No. Alloy grades studied Rating based on corrosion resistance Refs.
1 740, 263, 617 740 > 263 > 617 [18]

2 740, 740H 740H > 740 [17]

3 617, 617B 617B > 617 [22]

4 740H, 263, 617 740H > 263 > 617 [10]

Table 7. Relative rating of candidate superalloy grades from the point of view of hot corrosion in simulated USC power
plants.
Hot Corrosion of Superalloys in Boilers for Ultra-Supercritical Power Plants 35
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7. Mechanisms of hot corrosion of superalloys in USC power plants

7.1. Initiation and propagation of hot corrosion reaction

From the studies carried out in the past, it emerges that hot corrosion reaction occurs in two
phases. In the first phase, referred to as initiation phase, there is essentially no weight change,
and the chromium oxide layer formed on the surface is still protective in nature. In the second
phase, referred to as propagation phase, the chromium oxide layer gets fluxed and loses its
protective nature. Degradation of the material starts, manifesting itself as a loss in weight. It is
often considered that extent of initiation phase is the safe regime for deploying the material in
service facing such hot corrosion conditions. If the corrosive environment is more aggressive,
the initiation phase may get reduced and propagation phase may take off earlier. For exam-
ple, compared to simulated coal ash environment, (simulated coal ash + flue gas) environ-
ment is more aggressive; in the latter environment, initiation phase was found to be shorter,
propagation phase taking off earlier [23]. Figure 1 schematically illustrates these issues.

7.2. Effect of chemical composition

7.2.1. Effect of chromium level

Gagliano et al. [26] carried out studies on 19 alloys varying in chromium content from 16 to
44% and concluded that material’s resistance to coal ash corrosion is primarily dependent
on chromium content, with alloys containing greater than 22% chromium generally exhibit-
ing satisfactory corrosion resistance. According to the rule of thumb in boiler construction
industry, with increasing chromium content in the alloy matrix, lower corrosion rates are
expected due to higher ability of sufficient diffusion barrier formation [27]. Based on hot cor-
rosion studies carried out on a number of special steels and superalloys, it was observed that
weight loss due to hot corrosion decreases with increasing chromium content. This is shown
schematically in Figure 2. This tendency appears to be true for iron-based austenitic alloys, as
confirmed within the COORETEC study [28, 29]. But for nickel-based austenitic alloys, this
tendency cannot be confirmed when SO2/SO3-rich atmospheres were present. Both grades 617
and 263 have similar chromium content; however, they perform very differently in SO2/SO3-
rich environment. Even though chromium content of alloy 617 is high lying at 22%, the oxide
scale is apparently not capable of forming a diffusion barrier tight enough to protect metal
against sulfur-induced corrosion [18].

7.2.2. Effect of cobalt

Cobalt is less resistant to hot corrosion than nickel. Nickel-based alloys are in general more
resistant to low-temperature hot corrosion than cobalt-based alloys. For example, Tiwari [30]
studied the relative hot corrosion behavior of a nickel-based superalloy and a cobalt-based
superalloy in Na2SO4-60% V2O5 environment at 900°C and reported that the latter had inferior
corrosion resistance.

Zhao et al. [15] reported the hot corrosion reaction in superalloy 740 propagated by the out-
ward migration of Cu and the inward migration of SO3. With the progressive formation of
36 Superalloys for Industry Applications

Figure 1. Schematic showing the initiation and propagation phases in the hot corrosion process.

Cr2O3 scale, there is an increase in Cr-depletion and enrichment of Co and Ni in the layers
immediately below the scale. Due to the high diffusivity of Co in the scale, CoO forms on the
exterior of the scale. CoO is surrounded by Cr2O3, and the solid-state reaction occurs to form
CoCr2O4 spinel in the outer of the scale gradually. CoO forming on the surface layer reacts
with SO3 to form CoSO4. Even though NiO may form on the surface and NiSO4 formation
could result through the reaction of NiO and SO3, it is believed that CoSO4 forms preferen-
tially due to the fact that CoSO4 is much more stable thermodynamically than NiSO4. The
dissolution of Co and CoO induces severe low-temperature hot corrosion. It may be noted in
this context that some candidate superalloy grades have considerable Co level in the chemical
composition. For example, superalloy 740 has as much as 19–20 wt% Co, and alloy 617 has
10–11 wt% Co. Zhao et al. [15] suggested that a decrease in Co level of the superalloy 740 will
act in a beneficial way to resist coal ash/flue gas corrosion. Further studies are required to
evaluate the effect of a decrease in the level of Co on the hot corrosion behavior of alloy 740.

7.2.3. Effect of molybdenum

Catastrophic or self-sustaining rapid hot corrosion can occur in superalloys, which contain
molybdenum because molybdenum oxide can react with Na2SO4 in the salt [31]. The effect
of Mo on hot corrosion of superalloys was reported [32–35]. The alloy containing Mo suffers
catastrophic degradation. It is reported that MoO2 reacts with Na2SO4 to produce an acid salt
(SO2-rich), leading to acidic fluxing. The MoO3 may get incorporated into the Na2SO4 via the
formation of complex compounds such as Na2MoO4, Na2MoO4.MoO3, and Na2MoO4.2MoO4.
Hot Corrosion of Superalloys in Boilers for Ultra-Supercritical Power Plants 37
http://dx.doi.org/10.5772/intechopen.76083

All these phases are liquid and have a high solubility of Al2O3 and Cr2O3. It may be noted in
this context that some of the candidate superalloys have significant levels of Mo. For example,
alloy 617 has as much as ~9 wt% Mo in its chemical composition.

7.3. Effect of temperature

Operating temperature is one of the important factors that influence sulfidation tendency
in coal ash hot corrosion of nickel-based superalloys [5]. A high sulfidation tendency can
be observed at low temperatures due to the formation of low-melting alkali sulfate eutectic
mixtures [5]. This is the reason why Ni-based superalloys suffer rapid degradation in the tem-
perature range of the so-called Type II hot corrosion. But, the sulfidation tendency decreases
at the high-temperature form of hot corrosion, in the temperature of the so-called Type I hot
corrosion. Extent of hot corrosion of Inconel 740 was found to be an important function of the
temperature in the temperature range of 700–800°C studied by the authors. The corrosion rate
was well in the acceptable range at 700°C. There was a 10-fold increase in the rate on increas-
ing the temperature to 750°C, and this was associated with large-scale internal sulfidation
and TiS formation. The corrosion rate at 800°C was lower than at 750°C, and the extent of TiS
formation was also lower than at 750°C.
The course of corrosion reaction can change with operating temperature. For Ni-XCr-10Al
alloy, corrosion follows a multistage parabolic rate law at 700°C, but it changes to a quasipa-
rabolic rate at 800°C [36].

Zhao et al. [15] studied the hot corrosion of alloy 740 at 550 and 700°C. Molten sulfate-induced
hot corrosion did not occur at 550°C since the sulfates on the coal ash do not melt at this

Figure 2. Schematic of the dependence of weight loss due to hot corrosion at 650°C on Cr content based on data obtained
for various special steels and superalloys.
38 Superalloys for Industry Applications

temperature. At 700°C, due to the formation of low-melting point eutectic, molten sulfates
form and cause accelerated attack after about 1000 h of exposure. No internal sulfidation
occurred at 550°C, while sulfides precipitated at scale/alloy interface and in Cr-depletion zone
at 700°C. The spinel phases occur in corrosion product at 700°C, while at 550°C that was not
the case.

7.4. Effect of aggressive species in the environment

The type and extent of hot corrosion are a function of the composition of flue gas, particularly
its SO2 content [19]. It has been demonstrated that the extent of hot corrosion of Inconel 740 in
the flue gas with SO2 was higher than that in the flue gas without SO2 [19]. The extent of sul-
fidation attack was much higher in the flue gas with SO2. SO2 in flue gas accelerated the cor-
rosion damage of the alloy in coal ash environment. The metal loss was found to be doubled
after 123 h of exposure on switching over from flue gas without SO2 to flue gas with 1% SO2.
The sulfidation was predominant in the propagation stage.

8. Conclusion

The subject of hot corrosion of superalloys in coal-fired boilers in advanced power plants is
a highly complex phenomenon, with a large multiplicity of variables coming into picture.
The chemical composition of the alloy plays an important role in this context. High levels
of cobalt and molybdenum may have a detrimental effect. While high levels of chromium
were found to be useful in combating hot corrosion, a simple relationship between chro-
mium level and resistance to hot corrosion does not seem to hold good when environments
contain sulfur-bearing species. Clearly, further work is warranted to optimize the chemical
composition to combat hot corrosion while maintaining the stress rupture strength and
microstructural stability over long periods of power plant operation. Increasing levels of
sulfur-bearing species in the environment increase the extent of sulfidation and suscepti-
bility to hot corrosion. Temperature is also an important parameter in influencing the hot
corrosion process; the progress of corrosion reaction and the phases present in the corro-
sion product could be very different, depending on the reaction temperatures.

Author details

Nageswara Rao Muktinutalapati1, Arivazhagan Natarajan1 and Moganraj Arivarasu2


*Address all correspondence to: m.nageswararao@vit.ac.in

1 School of Mechanical Engineering, Vellore Institute of Technology, Vellore, India

2 Center for Innovative Manufacturing Research, Vellore Institute of Technology, Vellore,


India
Hot Corrosion of Superalloys in Boilers for Ultra-Supercritical Power Plants 39
http://dx.doi.org/10.5772/intechopen.76083

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[31] Sidhu TS, Agrawal RD, Prakash S. Hot corrosion of some superalloys and role of
high-velocity oxy-fuel spray coatings—A review. Surface and Coatings Technology.
2005;198:441-446

[32] Pettit FS. Oxidation and Hot Corrosion of Superalloys. Warrendale, PA: The Metal
Society AIME; 1984. p. 651

[33] Misra AK. Mechanism of Na2SO4-induced corrosion of molybdenum containing nickel-


base superalloys at high temperatures I. Corrosion in atmospheres containing only.
Journal of the Electrochemical Society. 1986;133:1029-1038

[34] Peters KR, Whittle DP, Stringer J. Oxidation and hot corrosion of nickel-based alloys
containing molybdenum. Corrosion Science. 1976;16:791IN1797-796IN11804

[35] Fryburg GC, Kohl FJ, Stearns CA. Chemical reactions involved in the initiation of hot
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alloys at 700-800°C. Acta Metallurgica Sinica. 2011;47:1026-1031
DOI: 10.5772/intechopen.76085

Provisional chapter
Chapter 4

Ultrasonic
Ultrasonic Assisted
Assisted Machining
Machining of
of Nickel-Based
Nickel-Based
Superalloy
Superalloy Inconel
Inconel 718
718

Yongbo Wu, Qiang Wang,


Yongbo Wu, Qiang Wang, Sisi Li
Sisi Li and
and Dong Lu
Dong Lu

Additional information
Additional information is
is available
available at
at the
the end
end of
of the
the chapter
chapter

http://dx.doi.org/10.5772/intechopen.76085

Abstract
Inconel 718 has been widely used in industries because of its excellent mechanical prop-
erties. However, the machining process, particularly the turning/grinding, of Inconel
718 is still costly due to high cutting force and heavy tool damage. Fortunately, a prom-
ising material removal technique, that is, ultrasonic-assisted turning/grinding (called
UAT/UAG for simplicity), could potentially play a great role in the high efficiency pre-
cision machining of Inconel 718 due to its excellent features such as smaller turning/
grinding force, better surface quality, longer tool working life and lower heat genera-
tion. However, few attempts have been done on UAT/UAG of Inconel 718. Therefore,
in this work, in order to confirm the feasibility of machining Inconel 718 by UAT/UAG,
experimental apparatus/equipment has at first been constructed by installing an ultra-
sonic cutting-unit/spindle on a NC lathe/surface grinder for UAT/UAG operations,
and then experimental investigations have been performed to elucidate the fundamen-
tal machining characteristics involving Inconel 718 workpiece including the effects of
the ultrasonic vibration and the cutting/grinding speed on the work-surface finish, the
machining force and temperature, the chip formation, the tool/wheel wears and so on.
The obtained results show that grinding forces and surface roughness were decreased
in UAT/UAG.

Keywords: Inconel 718, machining, turning, grinding, ultrasonic vibration, surface


roughness, material removal, chip formation

1. Introduction

Inconel 718, a nickel-based superalloy, exhibits desirable properties over a wide tempera-
ture range and is widely used in aerospace, petroleum and nuclear industries because of

© 2016 The Author(s). Licensee InTech. This chapter is distributed under the terms of the Creative Commons
© 2018 The Author(s). Licensee IntechOpen. This chapter is distributed under the terms of the Creative
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Commons Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use,
distribution, and reproduction in any medium, provided the original work is properly cited.
distribution, and reproduction in any medium, provided the original work is properly cited.
44 Superalloys for Industry Applications

its excellent mechanical properties such as high fatigue strength, good corrosion resistance
and strong creep resistance [1]. In power generation equipment manufacturing industries
including gas turbine engines, most of Inconel 718-made products are commonly machined
by turning, cutting, milling and grinding. However, the excellent mechanical properties of
Inconel 718 are leading to high cutting force, severe work-surface damage and heavy tool
wear in conventional machining/finishing processes [2]. Especially, the turning/grinding pro-
cess (hereinafter called CT/CG for simplicity) of Inconel 718 is still costly due to the heavy and
rapid wear of tools.
As a promising material removal technique, ultrasonic-assisted turning/grinding (hereinafter
called UAT/UAG for simplicity) has attracted great attention for decades for the sake of its
excellent features such as smaller turning/grinding force, higher material removal rate, better
surface quality, longer tool working life and lower heat generation compared with those in
CT/CG [3–7]. However, in the most of conventional UAT processes, a linear ultrasonic vibra-
tion is applied only in a single direction [8–12], which leads to the difficulty in the obtainment
of a reasonable material removal rate especially for difficult-machine metal such as Inconel
718. On the other hand, in conventional UAG processes, most of researches have ever focused
mainly on the hard-brittle materials such as crystal silicon and ceramics [13–19], and few
attempts have been done involving Inconel 718.
Therefore, the present authors proposed a novel UAT technique in which an elliptical ultra-
sonic vibration generated by the synthesis of two orthogonal linear ultrasonic vibrations is
applied on the tool in the base plane and experimentally confirmed its performance in the
turning of Inconel 718 [20, 21]. This new method is hereafter called as EUAT. In addition, the
UAG of Inconel 718 in which a linear ultrasonic vibration is imposed to the grinding wheel
along the wheel axis was also attempted, and some significant results were attained [22, 23]. In
this chapter, the processing principles of EUAT/UAG and the respective corresponding appa-
ratuses are described. Then, the fundamental machining characteristics obtained are detailed.

2. Elliptical ultrasonic-assisted turning of Inconel 718

2.1. Processing principle and apparatus

The processing principle of elliptical ultrasonic-assisted turning (EUAT) is as illustrated in


Figure 1; an elliptical ultrasonic vibration is imposed on the cutting tool in the base plane
(XOY plane) and the workpiece is rotated at a speed nw around its own axis (X-axis) in addi-
tion to a feed motion of the cutting tool in X-direction at a feed rate vf and a depth of cut ap.
The elliptical ultrasonic vibration is achieved by the synthesis of two vibrations in X- and
Y-directions with the respective amplitudes of Ax and Ay generated simultaneously by the
ultrasonic vibration unit.
For realizing the processing principle, an experimental apparatus was constructed by
installing a commercial ultrasonic vibration unit (UL40-A1 by Takesho Co., Ltd.) onto the
Ultrasonic Assisted Machining of Nickel-Based Superalloy Inconel 718 45
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Figure 1. Processing principle of EUAT.

tool post of a commercial CNC lathe (TAC-360 by Takizawa Co., Ltd.) as shown in Figure 2.
A power supplier was used to apply an AC voltage into the ultrasonic unit for inducing
the ultrasonic vibration. A commercial dynamometer was fixed below the ultrasonic unit
to measure the cutting forces. As the tool, a coated carbide insert, which is installed at the
tip of the ultrasonic unit, was employed. The cutting temperature was measured using an
infrared camera.

For quantitatively confirming the generation of elliptical vibration, the vibrations of tool cutting
edge in X- and Y-directions were simultaneously measured by two laser Doppler vibrometers
(LV-1610; Ono Sokki Co., Ltd.). The frequency of the AC voltage was set at 40.9 kHz, based on
the given specification of the ultrasonic unit. Figure 3 plots the vibration amplitudes of the tool
cutting edge, Ax in X-direction and Ay in Y-direction, at different power supplying levels. It is
evident that as the power supplying increases, the values of Ax and Ay increase linearly to 2.35
and 2.05 μm, respectively, at the power level of 40%. Using the vibrations measured in both
directions, the trajectory of the tool cutting edge was captured by an oscilloscope (WaveJet 314;
LeCroy Co., Ltd), and the obtained trajectories for different power supplying levels were also
exhibited in Figure 3. Clearly, the tool cutting edge follows a clockwise elliptic motion, and the
46 Superalloys for Industry Applications

Figure 2. Apparatus for EUAT.

Figure 3. Effect of power supplying level on vibration amplitude.


Ultrasonic Assisted Machining of Nickel-Based Superalloy Inconel 718 47
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shape of ellipse remains essentially unchanged with a declined angle of 168° even the power sup-
plying level varied, but the size of trajectory increased as the power supplying level escalated.

2.2. Machining conditions and procedure

Table 1 summarizes the machining conditions in experiments. As the workpiece, an Inconel


718 rod with the dimension of 40 mm in diameter and 100 mm in length was used. The cut-
ting speed vc was hence changed from 75 m/min to 125 m/min when the workpiece rota-
tional speed nw was adjusted from 600 to 1000 rpm. During machining, the cutting forces and
the cutting temperature were measured using the three-component dynamometer and the
infrared camera, respectively. After machining, the work-surface roughness was evaluated by
using a surface profiler (Talysurf Intra by Taylor Hobson Inc.), and the surface morphology of
workpiece was captured by using a laser microscope (VK-8710 by Keyence Co., Ltd). In addi-
tion, for comparison, the conventional turning (CT) operations were also conducted on the
same experimental apparatus but turned off the power supplier to set the power supplying
level at 0%, that is, Ax = Ay = 0.

2.3. Fundamental machining characteristics

Cutting force and temperature. In order to confirm that the ultrasonic vibration-reducing effect
of cutting force (UREF) still exists in the high speed cutting of Inconel 718 when EUAT is per-
formed in the base plane, the effect of cutting speed on cutting force in CT and EUAT was studied
by experiments. The results are presented in Figure 4, demonstrating that in comparison with
CT with EUAT, when the cutting speed was 75 m/min, the feed force Fx, the radial force Fy and
the cutting force Fz were reduced by 38%, 46% and 25%, respectively. Similarly, even the cutting
speed was increased to 87.5 m/min, then 100 m/min, further 112.5 m/min and finally 125 m/min,
similar reduction percentages were observed on the Fx, Fy and Fz with those at 75 m/min.

In other words, even when the cutting speed goes beyond the maximum ultrasonic vibration
velocity of πfAp-p, UREF is barely affected by the increase in the cutting speed. This may be

Workpiece Inconel 718 (ϕ 40 mm × L 100 mm)

Cutting tool Coated carbide

Normal rake angle α = 0 (°)

Normal clearance angle γ = 11 (°)

Nose radius rn = 0.4 rn(mm)

Cutting parameters nw = 600–1000 (rpm) (vc = 75–125 m/min), vf = 0.05 (mm/rev), ap = 0.05 (mm)

Ultrasonic vibration In CT: Ax = Ay = 0

In EUAT: f = 40.9 kHz, Ax = 2.07 μm, Ay = 2.81 μm, declined angle: 168°

Coolant Dry cutting

Table 1. Machining conditions in EUAT of Inconel 718.


48 Superalloys for Industry Applications

because the ultrasonic separation exists between the tool nose and the workpiece in X- and
Y-directions in the base plane, respectively, in EUAT. In addition, in both CT and EUAT, the
largest force was Fy, followed by Fx and Fz in descending order [24].

The cutting temperatures at different cutting speeds in CT and EUAT were also obtained as
shown in Figure 5. The results demonstrated that either in CT or in EUAT, as the cutting speed
increased, the cutting temperature rose monotonously; however, the increase rate in EUAT
seemed consistently lower than that in CT, indicating the ultrasonic vibration significantly
contributed to the reduction of cutting temperature in turning Inconel 718.
Chip morphology. Figure 6 shows that the chip width in EUAT is smaller than that in CT,
indicating that the chip morphology is affected by the cutting forces; the increase in cutting
force adds the transverse flow of the material, leading to an increase in the chip width [25].
Moreover, the adhesion of microchips can be observed evidently on the chip surface in CT,
which can hardly be seen in EUAT. These phenomena may be connected to the formation of
BUE (built-up edge) during cutting, which will be discussed in the “Tool Wear” section.
Work-surface finish. The surface morphologies of workpieces machined by CT and EUAT at
three different cutting speeds of 75, 100 and 125 m/min were captured by the laser microscope.
From the microscopic images shown in Figure 7(a), it is found that regardless of the cutting speed,
obvious parallel cutting traces and randomly distributed pits can be observed on the work-surface
in CT; the phenomena may be attributed to the formation of BUE on the cutting tool and chip
winding during cutting. By contrast, in EUAT (Figure 7(b)), knitted work-like texture was formed
on the work-surface owing to the tool vibration, and the work-surface integrity became better.
This is probably attributed to the fact that the chips were no longer wrapped around workpiece
and easily broken for the sake of the elliptical vibration of cutting tool in the base plane.

Figure 4. Effect of cutting speed on cutting forces.


Ultrasonic Assisted Machining of Nickel-Based Superalloy Inconel 718 49
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Figure 5. Effect of cutting speed on cutting temperatures.

Figure 6. SEM micrographs of chips developed in CT and EUAT methods: (a) in CT and (b) in EUAT.

The work-surface roughness was measured in the feed direction using the surface profiler for
both CT and EUAT. The evaluation length was set to 5 mm. In each test, the surface roughness
parameters Ra and Rz were measured eight times, and their average values were calculated and
regarded as the roughness. Figure 8 shows the effect of the cutting speed on the work-surface
roughness in CT and EUAT at three different cutting speeds of 75, 100 and 125 m/min. The
surface roughness Ra and Rz in EUAT seemed both larger than those in CT. In EUAT with the
increase of cutting speed, the Ra and Rz slightly decreased, while in CT, the Ra and Rz tended
to increase slightly which is caused by the formation of built-up edge (BUE) on tool cutting
edge [20].
Tool wear. Figure 9(a) and (b) shows the SEM images of the cutting edge of tool employed
for 4.2 min in CT and EUAT, respectively. Evidently, in CT, the BUE appeared on the cutting
50 Superalloys for Industry Applications

Figure 7. 2D laser microscopic images of the work-surfaces machined: (a) in CT and (b) in EUAT.

Figure 8. Effect of cutting speed on work-surface roughness.

tool, whereas in EUAT, it was absent. Comparing Figure 9(a) with Figure 9(b) shows that the
cutting tool adopted in CT experienced considerably heavier flank wear than that adopted in
EUAT. The maximum flank wears in CT and EUAT were 0.23 and 0.19 mm, respectively. This
indicates that the cutting tool was worn down more rapidly in CT than in EUAT, possibly
because the tool vibration in EUAT reduces the friction between the tool and the workpiece.
In EUAT, the ultrasonic vibration of tool occurs simultaneously in X- and Y-directions and
Ultrasonic Assisted Machining of Nickel-Based Superalloy Inconel 718 51
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Figure 9. SEM images of cutting tools used in (a) CT and (b) EUAT for 4.2 min (power supply level = 20%).

results in a clockwise elliptical motion in the base plane (see Figure 1). During cutting, owing
to the elliptic vibration the tool repeats the cutting-in and cutting-out action periodically. This
action reduces the formation of BUE and eventually retains the sharpness of the tool cutting
edge. Therefore, the chips and the work-surface in EUAT are almost free of chip particles.

3. Ultrasonic-assisted grinding of Inconel 718

3.1. Processing principle and equipment

The processing principle of UAG is illustrated in Figure 10; an axial ultrasonic vibration is
imposed on the grinding wheel in x-direction and the workpiece is fixed on a work-holder
under which a z-stage is located for determining the wheel depth of cut Δ. The peripheral
speed of grinding wheel is Vc and a feed motion is given to the workpiece in y-direction.
For comparison, a conventional grinding (CG) was also performed by releasing spindle from
ultrasonic vibration (Figure 11).

Figure 10. Processing principle of ultrasonic-assisted grinding.


52 Superalloys for Industry Applications

For realizing the processing principle, an experimental apparatus was constructed by install-
ing a commercial ultrasonic vibration spindle (URT40 by Takesho Co., Ltd., Japan) onto a
commercial NC grinder (GRIND-X IGM15EX by Okamoto Machine Tool Co., Ltd., Japan).
A commercial dynamometer (9256A by Kistler Co., Ltd., Switzerland) was positioned under
the ultrasonic spindle. On the lower end of the spindle, a metal-bonded #140 cBN grinding
wheel with a diameter of ds = 8 mm was fixed and an Inconel 718 specimen (L48 mm×W36
mm×T3 mm) was used as the workpiece. The abrasive grains on the working surface of the
wheel employed were observed by a three-dimensional (3D) SEM (ERA-8900 by ELIONIX. Co.,
Ltd., Japan), showing that most of the grains were cone shaped and their vertical angles and
average diameter were around 120° and 105 μm, respectively.

3.2. Grinding conditions and procedure

Table 2 exhibits the grinding conditions. As the purpose of this work is predominantly to
reveal the fundamental machining characteristics in UAG of Inconel 718 including the effects
of the ultrasonic vibration and the wheel peripheral speed on the grinding force and specific

Figure 11. Photo of equipment for ultrasonic-assisted grinding.

Workpiece Inconel 718, L48 mm × W36 mm × T3 mm

Grinding wheel Electroplated cBN#140, ϕ8 × L8 mm (FSK 140)

Ultrasonic vibration Frequency f = 40 kHz

Amplitude AP-P = 0–9.4 μm

Process parameters Workpiece feed rate Vw = 15 mm/min

Wheel peripheral speed Vc = 100.5–138.2 m/min (wheel rotational speed ng = 4000–5500 rpm)

Grinding width b = 3 mm

Wheel depth of cut ∆ = 80 μm

Coolant Without (dry grinding)

Table 2. Grinding conditions.


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grinding energy, the work-surface finish, the chip formation (chip size and geometry), the
material removal rate and the grinding wheel wear, the grinding operations were performed
at different ultrasonic vibration amplitudes and wheel peripheral speeds but the constant
workpiece feed rate and wheel depth of cut.

Typically, cBN abrasives require a cutting speed of over 50 m/min for grinding Inconel 718
[16]. Therefore, the value of wheel peripheral speed Vc was set at 100.5–138.2 m/min (wheel
rotational speed ng = 4000–5500 rpm). In order to ascertain the benefits from application
of the ultrasonic vibration to precision grinding, the workpiece feed rate was set at a low
value of 5 mm/min. Correspondingly, a large value of depth of cut is required to ensure
material removal rate; hence, the value of Δ was set at 80 μm. The actual vibration ampli-
tude Ap–p of the wheel was measured using the Laser Doppler vibrometer (LV-1610 by On
Sokki Co., Ltd., Japan), revealing that the value of Ap–p was varied in a range of 0–9.4 μm
as the power supplying level rises. In addition, dry grinding operations were performed
without coolant supplying.

The material removal rate Q was also experimentally obtained using the relationship of
Q = bΔrVw, where Δr is the actually measured work-depth removed. Furthermore, the ground
work-surface roughness was measured with the surface profiler (Talysurf Intra by Taylor
Hobson Inc.) to indicate the work-surface finish. For further investigation, the chips used for
the SEM observation were those escaped out of the grinding zone during dry grinding and
collected by a piece of conductive plastic (4⨯4 mm), which was located nearby the grinding
zone. The working surface condition of grinding wheel, that is, the chips adhesion, the wheel
wear behavior like grain releasing/fracture were also examined by SEM observation.

3.3. Fundamental grinding characteristics

Grinding force, specific grinding energy and material removal rate. Figure 12(a) and (b)
shows the grinding forces measured under various values of Ap-p and Vc, respectively. Evidently,
either the tangential force Fy or the normal one Fz monotonously decreased as the Ap-p increased
(Figure 12(a)), and almost linearly decreased with the increasing Vc (Figure 12(b)). It should
be noticed, for example, that at Vc = 138.2 m/min, once the ultrasonic vibration at Ap-p = 9.4 μm
has been applied, the values of Fy and Fz were dropped by 51.9% and 38.6%, respectively, com-
pared with that without ultrasonic vibration (Ap-p = 0 μm). Additionally, considered that the
Fz affects tremendously, the formation of micro fracture defects on chip which is character-
ized by the knife chip, a lower Fz in UAG might lead to a smaller number of knife chips (see
Figures 18 and 19) compared with that in CG.

In addition, the grinding force ratio of Fz/Fy was obtained as exhibited in Figure 12, showing
that the ratio increased with the increasing Ap-p (Figure 12(a)), whereas little effect of the Vc
can be observed on the ratio (Figure 12(b)) either in CG or in UAG. As revealed by Dong Kun
Zhang [26], the lower friction ploughing and smaller chip deformation lead to the increase
of grinding force ratio. Therefore, the results demonstrated that ultrasonic vibration contrib-
uted to the reduction of friction ploughing and chip deformation. Further, a larger vibration
amplitude seemed to increase the material removal ratae, as shown in Figure 13. This con-
firmed that the ultrasonic vibration can enhance the material removal owing to the decrease
in grinding forces.
54 Superalloys for Industry Applications

Figure 12. Effects of (a) vibration amplitude and (b) wheel peripheral speed on grinding forces.

Figure 13. Effects of vibration amplitude on material removal rate.

Furthermore, the specific grinding energy, u, in UAG was compared with that in CG. As the u
is defined as the energy per unit volume of material removed [27], it can be expressed in Eq.
(1) in CG and Eq. (2) in UAG, respectively.

u = Fy Vc / 1000bΔ Vw (1)

u = (Fy Vc + Fx Vx) / 1000bΔ Vw (2)

where Fx (N) is the grinding force in x-direction due to the wheel ultrasonic vibration and Vx
(m/min) is the wheel ultrasonic vibration speed determined by the equation of
Ultrasonic Assisted Machining of Nickel-Based Superalloy Inconel 718 55
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Vx(t) = 2π fAp−p cos (2𝜋𝜋ft) (3)

Both of them are varied periodically at the frequency of f during grinding.

In the current work, the values of Vc, b, Δ and Vw have been already known as exhibited in
Table 2 and that of Fy is also the already known one as shown in Figure 12. The measured
results of Fx and the calculated value of Vx are given in Table 3. The FxVx changed from 0
to the respective peek values for different Ap-p, while the FyVc decreased with the increase
of Ap-p.

Figure 14 shows the relation between u and Ap-p. It can be seen from this figure that although
the u varied between uL and uH at the given Ap-p for the sake of the ultrasonic vibration, the u
intended to decrease as the Ap-p increases, confirming that the ultrasonic vibration benefits the
reduction in the specific grinding energy significantly.

Work-surface finish. Given that the effective cutting edge distribution density affects the
work-surface roughness in grinding processes and that this density is affected by the ultra-
sonic vibration [22], it was also investigated how the work-surface finish varied with vibra-
tion amplitude Ap-p. Figure 15 shows the obtained results, demonstrating that the ultrasonic

Ap-p (mm) 0 2.2⨯10−3 4.1⨯10−3 5.8⨯10−3 7.7⨯10−3 9.4⨯10−3


Vx (m/min) 0 −16.6–16.6 −30.9–30.9 −43.7–43.7 −58–58 −71–71

Fx (N) 0 −0.1–0.1 −0.1–0.1 −0.1–0.1 −0.1–0.1 −0.1–0.1

FxVx 0 0–1.7 0–3.1 0–4.4 0–5.8 0–7.1

FyVc 718.6 552.8 483.7 428.4 387.0 345.5

Table 3. Vx, Fx, FxVx and FyVc typically obtained at Vc = 138.2 m/min for various values of Ap-p.

Figure 14. Effect of ultrasonic vibration on specific grinding energy.


56 Superalloys for Industry Applications

Figure 15. Effect of ultrasonic vibration amplitude on work-surface finish.

vibration indeed contributed to the work-surface finish improvement; the larger the Ap-p was,
the smaller the work-surface roughness became. The optical microscopic images of work-
surfaces in CG and UAG were also compared in the same figure, showing that on the work-
surface by CG only parallel grain cutting marks were formed, whereas on that by UAG, many
ultrasonic-induced knitting-patterned cutting marks overlap with the parallel ones.
Chips formed. An electron scanning microscope (SEM) with 3D measurement/observation func-
tions (ERA-8900 by ELIONIX Co., Ltd.) was employed to measure the 3D chip size and observe
the chip geometry. Figure 16(a) and (b) shows the 3D SEM images of chips formed in UAG
(AP-P = 9.4 μm) and CG at Vc = 138.2 m/min, respectively. The measured results of mean length
and cross section area of chips are shown in Figure 16 (c) and (d). It is evident in Figure 16(c)
that the ultrasonic vibration leaded to the reduction of mean length and mean cross section
area of chips. Especially, when the amplitude was Ap-p = 9.4 μm, the mean length was reduced
by 36.3% and the cross section area was reduced by 64.3%. Figure 16 (d) shows the effect of the
wheel peripheral speed Vc, demonstrating that as the Vc increases the cross section area intends
to reduce either with or without ultrasonic vibration, but the effect on the chip length was not
obvious.
In conventional grinding of Inconel 718, the formed chip could be classified into six types:
flow, shear, rip, knife, slice and melt [28]. In this study, all the six types occurred; however,
dominant types were shear, knife and flow either in CG or UAG as shown in Figure 17.
Further, the number percentages of each type under different conditions were experimentally
investigated, and the obtained results (Figure 18) show that the majority of chips in CG were
shear type, whereas most of them in UAG were flow type especially at larger vibration ampli-
tude (Ap-p ≥ 4.1 μm). This indicates that the UAG of Inconel 718 is potentially avoiding the
formation of shear chips and prefers the flow chips especially at larger amplitude.
As for the effect of the wheel peripheral speed Vc, it can be found from Figure 19 that in
CG when the Vc changed from 100.5 m/min to 113 m/min, the percentage of the flow chip
Ultrasonic Assisted Machining of Nickel-Based Superalloy Inconel 718 57
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Figure 16. Effects of ultrasonic vibration and wheel peripheral speed on chip size: (a) 3D SEM images of chips in UAG
at Ap-p = 9.4 μm, (b) 3D SEM images of chips in CG, (c) chip length and cross section area vs. vibration amplitude and (d)
chip length and cross section area vs. wheel peripheral speed.

increased from 4 to 63% and the change in the percentage of knife chip was very small, while
that of the shear chips reduced from 86 to 30%. As the increase of Vc the number percentage
of three types of chips were not obvious. In UAG, the increase of Vc was not main effect to the
change of number percentage of chips.

Working surface condition of grinding wheel. Through SEM observation, the working sur-
face morphologies of wheel with/without ultrasonic vibration were captured. From the SEM
images shown in Figure 20, it is found that both chips adhesion and grains releasing/fracture
occurred during grinding. Comparing the right sides of Figure 20(a) and (b) revealed dis-
tinctly that the ultrasonic vibration reduced both the chips adhesion and grains releasing/
fracture significantly.

Furthermore, the chips adhesion area was filtered, extracted and binarized by using Image-
Pro Plus for quantitative analysis [22]. For this purpose, an observation zone with size of
1.13 mm × 6 mm on grinding wheel working surface was selected to measure the percent-
age of chips adhesion area in the total wheel working surface area, as shown in Figure 21.
Obviously, increasing the ultrasonic amplitude leads to the reduction of the percentage of
chips adhesion area. Especially, at AP-P = 9.4 μm, a decrease by 72.4% was observed.
58 Superalloys for Industry Applications

Figure 17. Chips type: (a) shear chip in CG; (b) knife chip in CG; (c) flow chip in CG; (d) shear chip in UAG; (e) knife chip
in UAG and (f) flow chip in UAG, at ∆ = 80 μm and Vc = 138.2 m/min.

Figure 18. Effect of vibration amplitude on chip type.


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Figure 19. Effect of wheel peripheral speed on chip type.

Figure 20. SEM images of the grinding wheel working surfaces before (left sides) /after (right sides) grinding of Inconel
718 (a) without and (b) with ultrasonic vibration: (a) in CG at Ap-p = 0 μm and Vc = 138.2 m/min and (b) in UAG at
Ap-p = 9.4 μm and Vc = 138.2 m/min.
60 Superalloys for Industry Applications

Figure 21. Effects of vibration amplitude on the percentage of chips adhesion area.

Figure 22. Effect of vibration amplitude on the percentage of grain releasing/fracture number.

At last, the releasing/fracture of abrasive grains was investigated by comparing the percent-
ages of grain releasing/fracture number in total wheel working surface in CG and UAG, as
shown in Figure 22. It is noticed that in CG (Ap-p = 0 μm), the percentage reached 44%. Once an
ultrasonic vibration with a small amplitude of Ap-p = 2.2 μm has been imposed, the percentage
turned to be less than 20%, demonstrating that the presence of ultrasonic vibration restraints
Ultrasonic Assisted Machining of Nickel-Based Superalloy Inconel 718 61
http://dx.doi.org/10.5772/intechopen.76085

the grain releasing/fracture phenomenon considerably. In addition, when compared the CG


result with the UAG one at Ap-p = 9.4 μm, it is figured out that the percentage decreased by
40%. This phenomenon is attributed to the ultrasonic vibration-induced vertical inertia force
which acts on chips. This vertical inertia force encourages chips to leave cutting edge and
hence increases cutting capacity of grain.

4. Summary

As a step toward the development of a novel technique for the machining of superalloy
Inconel 718, at first the elliptic ultrasonic-assisted turning (EUAT) method was proposed and
its fundamental performance was experimentally confirmed, then the ultrasonic-assisted
grinding of Inconel 718 was attempted and successfully elucidated the fundamental grinding
characteristics. The obtained results can be summarized as following.
In EUAT, (1) the cutting force was considerably smaller than that in conventional turning (CT)
and strengthening the ultrasonic vibration decreased the cutting force; (2) although ultrasonic
vibration marks were formed on the work-surface along the cutting direction, the surface
finish was improved, whereas scratches and pits obviously existed on the work-surface in
CT and (3) the ultrasonic vibration significantly restrained the formation of built-up edge on
cutting tool and decreased the flank wear of tool.

In UAG, (1) imposing the ultrasonic vibration to the grinding wheel decreased the grinding
forces and increased the material removal rate significantly. Strengthening the wheel ultra-
sonic vibration decreased the specific grinding energy, demonstrating that the ultrasonic
vibration benefits the reduction in the energy consumption. (2) The ultrasonic vibration con-
tributed to the work-surface finish improvement; the larger the Ap-p was, the work-surface
roughness became better. (3) The chip size, that is, cross-section area and length, was distinctly
affected by the ultrasonic vibration but little effect of wheel peripheral speed is observed. (4)
The ultrasonic vibration in grinding is avoiding the formation of shear chips and prefers the
flow chips especially at larger amplitude. (5) The grinding wheel wear was dominantly attrib-
uted to chips adhesion, grains releasing/fracture which are reduced significantly by the ultra-
sonic vibration. The percentage of chips adhesion area and the number percentage of grains
released/fractured decreased as the vibration amplitude increased.

Author details

Yongbo Wu1,2*, Qiang Wang¹,2, Sisi Li¹,2 and Dong Lu2

*Address all correspondence to: wuyb@akita-pu.ac.jp

1 Akita Prefectural University, Akita, Japan

2 Southern University of Science and Technology, Shenzhen, China


62 Superalloys for Industry Applications

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DOI: 10.5772/intechopen.78669

Provisional chapter
Chapter 5

Dry
Dry High
High Speed
Speed Orthogonal
Orthogonal Turning
Turning of
of Titanium
Titanium Alloy
Alloy
Wear
Wear Evolution
Evolution and
and Chip
Chip Morphology
Morphology

Mohieddine Benghersallah, Lakhdar Boulanouar,


Mohieddine Benghersallah, Lakhdar Boulanouar,
Gautier List and Guy Sutter
Gautier List Guy Sutter

Additional information is available at the end of the chapter

http://dx.doi.org/10.5772/intechopen.78669

Abstract

The present work is an experimental study on the dry high-speed turning of Ti-6Al-4 V
titanium alloy. The objective of this study is to see for high cutting speeds, how wear
occurs on the face of insert and how to evolve cutting forces and chip formation. Cutting
speeds tested is 600, 800, 1000 and 1200 m/min in orthogonal turning with a carbide insert
tool H13A uncoated and coated TiN on a cylindrical titanium alloy part. Investigation on
the wear inserts with 3D microscope scanning revered the crater formation is instanta-
neous and a chip adhesion. Welded chip causes detachment of carbide particles. In these
experiments the chip shape was systematically investigated at each cutting conditions
using optical microscopy. The chips produced were collected and polished to measure
the thicknesses t2max and t2min. The distance between each segments dch and ɸseg inclina-
tion angle as described in the introduction part, the shear angle ɸ and the inclination
angle of a segment ɸseg are differentiated. ɸseg angle is actually measured on the col-
lected chips while the shear angle ɸ cannot be. The angle ɸ represents the initial shear
similar to the one that describes the formation of a continuous chip in the primary shear
zone. Cutting forces increase and stabilize before removing the tool. The chip reaches a
very high temperature.

Keywords: titanium alloys, dry high-speed machining, chip formation, cutting zone,
confocal imaging

1. Introduction

Titanium alloys such as Ti–6Al–4 V, Ti-555, Ti6242S, and Ti-LCB, are used extensively in the
aerospace industry for structural components (compressor blades, disks, castings, and gas

© 2016 The Author(s). Licensee InTech. This chapter is distributed under the terms of the Creative Commons
© 2018 The Author(s). Licensee IntechOpen. This chapter is distributed under the terms of the Creative
Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use,
Commons Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use,
distribution, and reproduction in any medium, provided the original work is properly cited.
distribution, and reproduction in any medium, provided the original work is properly cited.
66 Superalloys for Industry Applications

turbine engines) due to their superior properties such as excellent strength-to-weight ratio,
strong corrosion resistance and ability to retain high strength at high temperatures [1–3].
Light-weight materials such as titanium alloys are now used in modern aerospace structure
due to their best combination of metallurgical and physical properties. Each class of titanium
alloy has their advantages and disadvantages. Titanium’s advantages are high strength-to-
weight ratio, low density, excellent corrosion resistance, excellent erosion resistance and low
modulus of elasticity.

Ti-6Al-4 V may be considered in any application where a combination of high strength at


low to moderate temperatures, light weight and excellent corrosion resistance are required.
Some of the many applications where this alloy has been used include aircraft turbine engine
components, aircraft structural components, aerospace fasteners; high-performance automo-
tive parts, marine applications, medical devices, and sports equipment [1–4].

Titanium and its alloy have poor machinability, this may be due to their high chemical reac-
tivity with most cutting tools and therefore, have a tendency to weld to the cutting tool during
machining, thus leading to chipping and premature tool failure. Its low thermal conductivity
increases the temperature at the tool/work piece interface, which affects the tool life [2, 3, 5].

Minimum quantity lubrication (MQL) is widely applied for titanium alloy machining, mean-
while, in the machining process of titanium alloy, there are several problems regarding tool
wear, poor surface damage, and machining deformation. Moreover, surface damage usu-
ally appears during high-speed machining. Therefore, the contradiction between increasing
machining demand and machining performance has become a bottleneck in actual industry.

On the other hand, there are critical needs to reduce the usage of cutting fluid in machining
process in order to reduce the environmental burden and economic cost [3]. Dry and minimum
quantity lubrication (MQL) machining which are two types of green manufacturing processes
have vast potentials for machining of titanium alloys [4–6]. Additionally, the tool coating is
a key factor to realize high-speed machining and green manufacturing. Coating materials
is widely employed to extend tool life and cutting performance of cutting tools due to their
advanced wear resistance and superior performance under corrosive or high temperature
conditions. However, the tool coatings used presently in machining of titanium alloys cannot
meet with the need of high-speed machining and green manufacturing. Simultaneously, as
one of an effective green manufacturing technology, the combination of MQL and novel cut-
ting tools is also growing.

1.1. Topographic tool wear characterization

In recent years, many microscopy techniques were commonly used for characterizing the
surface topography in many scientific fields (Figure 1) [7, 14, 20].

The atomic force microscopy (AFM), stylus profilometry, stereo microscopy (SM), scanning
electron microscopy (SEM), reflected light interference microscopy (RLIM), and confocal laser
scanning microscopy (CLSM). The first two are touch instruments, while others are non-contact
instruments. AFM, the state of the art profiler, has excellent depth and transverse resolution.
Dry High Speed Orthogonal Turning of Titanium Alloy Wear Evolution and Chip Morphology 67
http://dx.doi.org/10.5772/intechopen.78669

Figure 1. General principle of surface characterization methods [7].

However, its disadvantages such as slow scan very small field sample (usually 70 × 70 um),
restricted depth range (about 5 μm), its inability to scan deep holes, and the extreme fragility
of the tip prevented its immediate application to tool wear analysis [8–11].
In the conventional optical microscope, the image is “flat”, providing lateral dimensional
information (X and Y), but not axial (Z). The image contrast is derived generally in variations
of surface reflectivity. Confocal microscopy provides quantitative information on the optical
axis (Z). The principle of the confocal microscope is to focus, through a goal, a laser beam will
illuminate a point of the sample, then recovering on a photomultiplier, the light signal emitted
at this point [12, 13].

Confocal microscopy is a non-destructive optical technique to obtain optical sections not


only in the plane (X, Y), but also along a plane (X, Z) parallel to the optical axis which can
be obtained a three-dimensional reconstructions [14]. These optical sections “virtual” do not
affect the entire sample unlike physical cuts necessary in electron microscopy. The latest
developments in fluorescent confocal microscopy allow, for marking means based on the use
of fluorescent products, observe remarkable 3D structures.

One of the drawbacks of confocal microscopy is its slow action. Indeed, the measurement of a
3D structure requires up to a few hours.

The principle of the operation of the confocal microscope is shown in Figure 2. Light emitted
from the source after passing through the optical path is focused on the analyzed surface.
The reflected beam reaches to a diaphragm which transmits only focused light and to a pho-
todetector. A vertical scanning system is moving the lens, which allows to analyze different
height areas of roughness. That ability to distinguish height improves significantly the con-
trast and the lateral resolution in comparison with the classic optical microscope. Scanning
confocal microscopes took advantage of the differentiation of depth and generating of surface
image and reception of reflected beam is done by the same optical system. Like in the scan-
ning method, the optical system generates a spot on a surface, and a reflected light beam is
recorded by a point detector. In the construction of a diaphragm of a modern confocal micro-
scope a Nipkow disk with a series of spiral splitting small holes is used. In connection with a
68 Superalloys for Industry Applications

Figure 2. Confocal microscopic principle [7, 15–17].

suitably prepared light beam (after passing through another Nipkow disk with microlenses)
it allows a scan of the surface topography effectively.

The scanning microscope in recent years has been generally accepted. It is a tested and
approved technique on the nano scale, which allowed to obtain very good vertical resolution.
Serious problems appear only in the case of very rough surfaces and the necessity to use a
larger vertical range. Microscope application can cause a little difficulty in the interpretation of
results of measurement, especially when samples have inclusions or impurities on the surface,
which characteristics are variable or can have an influence on response of instrument [14].

The cutting edge shape and the cutting edge condition are of crucial importance for machining
operations. During the cutting process the impact of high thermal and mechanical loads on the
cutting edge result in wear. Moreover, the quality of the machined surface is affected by the
cutting edge shape. The demands of modern production are high productivity and high pro-
cess reliability. One place these demands can be met is in cutting edge preparation [13, 14, 18].

Tool wear is one of the most complex problems in machining because it is affected by various
factors such as the behavior of the work material, the interaction of the work material with
the cutting tool, machining condition, dynamics, and the stability of machining tools. This
makes the identification of the dominating wear mechanisms very difficult. The development
of wear models based on these wear mechanisms, the interfacial stress and temperature fields
Dry High Speed Orthogonal Turning of Titanium Alloy Wear Evolution and Chip Morphology 69
http://dx.doi.org/10.5772/intechopen.78669

determination, and the topography characterization of tool wear stand out among the most
urgent issues in this area of research. If these issues can be resolved, tool life can be easily
predicted and the effectiveness of cutting tools improved.

Tool life is dictated by catastrophic failure, plastic deformation, and gradual wear. The first
two imply premature failures of a tool and, therefore, should be avoided at all times. Gradual
wear is the main interest because it limits tool life in a typical machining condition. The most
common forms of gradual tool wear are flank wear and crater wear. Flank wear limits the ser-
vice life of a tool directly because it affects dimensional accuracy, forces generated, and power
consumption. Crater wear can reduce the cutting forces. However, the weakening of the cutting
edge ultimately leads to failure. Crater wear represents a greater challenge than flank wear due
to many competing wear mechanisms, such as abrasion, dissolution, and/or diffusion [14, 18].

1.2. Tool wear mechanisms

For many years, the study of tool wear has been limited to empirical approaches. The well-
known empirical Taylor’s equation, for example, is convenient when dealing with few work
materials and cutting tools. However, it is unable to predict the performance of new work
and tool materials without a substantial amount of machining experiments. Therefore, such
an empirical equation cannot be used in the development of new cutting tools. On the other
hand, some researchers [13, 14, 19–24] have approached tool wear from physics-based models.

The main wear mechanisms involved in tool wear have been proposed to be adhesion, abrasion,
diffusion, and dissolution. Flank wear is caused mainly by abrasion of the hard second phase
in a work material. Crater wear is controlled by a combination of adhesion, abrasion, dissolu-
tion, and/or diffusion [15, 17, 25, 27, 29, 30]. At present, it is not clear exactly which mechanisms
dominate crater wear in relation to the cutting condition. In high-speed machining, crater wear
is believed to be dominated by dissolution wear and subsequent diffusion [15–17, 25–27]. The
aim of this paper is to explain qualitatively the high crater wear resistance of multilayer coated
carbides through the observation and analysis of their confocal topography.

2. Experimental work

The workpiece is a Ti–6Al–4 V alloy bar with a length of 300 mm and a diameter of 110 mm.
Tables 1 and 2 show the chemical composition and physical properties of the titanium alloy,
respectively.

The machining trials were carried out on a CNC lathe, with a 22 kW motor drive with a maxi-
mum torque of 2000 Nm. The spindle rotation speed ranges from 18 to 4500 rpm.

All cutting tests were carried out with uncoated carbide inserts (H13A-P15, 6% Co and 94%
WC) without chip-breaker, with a rake angle ˛ = 0° and a clearance angle of 7° [21].

The cutting forces were measured at the early stages of machining up to 1 minute, when the
inserts have not suffered appreciated wear, with a piezoelectric Kistler dynamometer (model
9441B), connected to a charge amplifier.
70 Superalloys for Industry Applications

Al V Fe O2 H2 N2 Ti
6 4 0.03 0.01 0.01 0.25 Balance

Table 1. Nominal composition of Ti-6Al-4 V (wt.%).

Tensile strength (MPa) 0.2% Proof stress (MPa) Density (g/cm3) Elongation
5D (%)
960 ± 1270 885 4.42 8

Reduction of area (%) Modulus of elasticity tension (GPa) Hardness Thermal conductivity
(Hv) (W/mK)

25 100–130 330–370 7

Table 2. Mechanical and thermal properties of Ti–6Al–4 V.

The tool inserts were used to machine the titanium alloy at the following conditions:
• Cutting speeds (m/min): 600, 800, 1000, 1200 m/min
• Feed rate (f): 0.1 mm/rev.
• Depth of cut: 3 mm
The test is to be machined orthogonally the workpiece on a depth ap = 0.3 mm and feed rate
f = 0.1 mm/rev. with five cutting speed values according (600, 800, 1000, 1200 m/min) (Figure 3).

Figure 3. Schematic diagram of experimental setup.


Dry High Speed Orthogonal Turning of Titanium Alloy Wear Evolution and Chip Morphology 71
http://dx.doi.org/10.5772/intechopen.78669

3. Results and discussion

A. Wear investigations

First investigations concerning the wear inserts to know if the H13A [28] tool material resists
wear for very high cutting speeds.

The microscope photography shows a welding chip on the rake face. The temperature in the
cutting zone reaches values near to the melting temperature of the material being machined.
Instantly the chip stands and removed with him the substrate material of the tool which
causes the crater wear.

Figure 4 shows the confocal image obtained by the microscope DCM3D of the cutting insert
for the machining conditions (V c = 600 m/min, f = 0.1 mm, ap = 3 mm) on this picture we
can see the welded chip on the rake face. Figure 4c), shows the profile diagram of the cutting
insert obtained by skew right A. A on unworn cutting edge and the profile of crater obtained
between welding chip zone by skew right B.B.

Figure 5a is a microscope photography of the cutting zone on the insert according the cutting
parameters (800 m/min, f = 0.1 mm/rev, ap = 3 mm) on the rake face we can see the crater wear
formation. Figure 5b shows 3D image of cutting insert according the cutting parameters, we
can see the crater wear formation in rake face and collapse of cutting edge. Figure 5c shows
the profile of crater wear obtained by skew right A.A.

Figure 4. (a) Photography of chip welding on rake face, (b) 3D confocal image of the cutting insert (600 m/min,
f = 0.1 mm/rev, ap = 3 mm), (c) profile diagram obtained by skew right unworn cutting edge and profile of crater failure
under chip welding.
72 Superalloys for Industry Applications

Figure 5. (a) Photography of cutting edge insert (b) 3D confocal image of the cutting insert according the cutting
parameters (800 m/min, f = 0.1 mm/rev, ap = 3 mm), (c) crater profile by skew right A.A.

Figure 6. (a) Photography of cutting zone of insert according the cutting parameters (1000 m/min, f = 0.1 mm/rev,
ap = 3 mm), (b) 3D confocal image, (c) profile 2D of crater wear.
Dry High Speed Orthogonal Turning of Titanium Alloy Wear Evolution and Chip Morphology 73
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The photography of optical microscope (Figure 6a) show the insert according the cutting
parameters (Vc = 1000 m/min, f = 0.1 mm/rev, ap = 3 mm). We can see the crater wear and chip
adhesion in different area. Figure 6b show in 3D image confocal the chip welded and crater
wear and the collapse at the sharp ridge. In Figure 6c, the crater wear values are defined with
the 2D profile.
The photography of optical microscope (Figure 7a) show the insert according the cutting
parameters (Vc = 1200 m/min, f = 0.1 mm/rev, ap = 3 mm). We can see the crater wear forma-
tion on rake face. Figure 7b, show in 3D image confocal the crater wear and the collapse at the
sharp ridge. In Figure 7c, the crater wear values are defined with the 2D profile.
Early investigations clearly show that for very high cutting speeds, the plate wears quickly.
This is due to excessive heating of the cutting area. The temperature in the cutting zone
reaches superior to the melting temperature of Ti-6Al-4 V values. This material known for its
poor thermal conductivity welds.

3.1. Confocal imaging of coated TiN insert

The confocal image of the Figure 8a shows a portion of the H13A TiN coating insert during
the cutting parameters (Vc = 600 m / min, f = 0.1 mm / rev, ap = 3 mm). On the flank face we
observed a welding chip of Ti6Al4V titanium alloy. The temperature in the cutting zone is
very high, the chip is welded, it causes wear in crater on the rake face. This crater is born
after the posting of the substrate particles forming the insert. The predominant wear is by
adhesion. The confocal image of the Figure 8b shows the wear on the H13A TiN coating insert

Figure 7. (a) Photography of cutting edge according (Vc = 1200 m/min, f = 0.1 mm/rev, ap = 3 mm). (b) 3Dconfocal image,
(c) profile 2D of crater wear.
74 Superalloys for Industry Applications

Figure 8. (a) 3D confocal image according (600 m/min, f = 0.1 mm/rev, ap = 3 mm) for coating TiN insert, (b) 3D confocal
image according (Vc = 800 m/min, f = 0.1 mm/rev, ap = 3 mm) for coating TiN insert.

for the cutting parameters (Vc = 800 m/min, f = 0.1 mm/rev, ap = 3 mm). On the rake face we
observed the crater wear formation caused by the adhesion of the titanium alloy chip. The
chip is welded and then migrates under the high-speed action of next chip. On the rake face
coating stands served and the increase in flank wear by abrasion to the total damage of the
cutting edge.
The confocal image of the Figure 9a shows the wear on the insert for the cutting speed
(Vc = 1000 m/min, f = 0.1 mm/rev, ap = 3 mm). The particles of the welding chip are observed.
Tearing of these chips causes a crater by wear adhesion. The chip welded titanium migrate
under the effect of the high-speed thrust next chip. On the flank face we observed the forma-
tion of the band of the flank wear and the effect of the temperature with the detachment of
the coating. The confocal image of the Figure 9b shows the wear on the coating insert for the
cutting parameters (Vc = 1200 m /min, f = 0.1 mm/rev, ap = 3 mm). On the rake face there is a

Figure 9. (a) 3D confocal image according (Vc = 1000 m/min, f = 0.1 mm/rev, ap = 3 mm) for coating TiN insert, (b) 3D
confocal image according (Vc = 1200 m/min, f = 0.1 mm/rev, ap = 3 mm) for coating TiN insert.
Dry High Speed Orthogonal Turning of Titanium Alloy Wear Evolution and Chip Morphology 75
http://dx.doi.org/10.5772/intechopen.78669

very pronounced crater wear caused by tearing of the chip that forces the particles from the
substrate to detach. The next chip and forms a crater wear. On the flank face we observed
the formation of the band of the flank wear and the effect of the temperature of the chip in
combustion phase leaving burn marks.

The overall analysis of 3D confocal images shows that the dominant wear for orthogonal
turning high-speed titanium is the main crater wear caused by adhesion.

3.2. 2D profiles of crater wear measurements

Figure 10 shows the profiles of the craters of each insert under different cutting conditions, we
can give the depth of each crater.

3.3. Diagram of crater wear evolution

Figure 11 shows the evolution of the depth of rake face crater for different parameters of
cutting regime and for the two types of inserts. With uncoated insert the largest depth of the
crater is recorded for 600 m/min testing. The depth of KT has decreased for 800 m/min cutting
speed, it increases significantly for 1000 m/min. At 1200 m/min we noticed a sharp decrease
in crater depth. For TiN coated insert, the value of the crater depth is substantially the same.
This is due to the coating which is a barrier against crater wear.

B. Flank wear characterization

In Figure 12 confocal image is observed from the flank face of the H13A TiN coating insert
following conditions:

Figure 10. (a) 2D profile of crater wear according the following conditions (Vc = 600 m/min, f = 0.1 mm/tr, ap = 3 mm). (b)
2D profile of crater wear according the following conditions (Vc = 800 m/min, f = 0.1 mm/tr, ap = 3 mm). (c) 2D profile of
crater wear according the following conditions (Vc = 1000 m/min, f = 0.1 mm/tr, ap = 3 mm). (d) 2D profile of crater wear
according the following conditions (Vc = 1200 m/min, f = 0.1 mm/tr, ap = 3 mm).
76 Superalloys for Industry Applications

Figure 11. Crater wear evolution for two carbides inserts according the cutting parameters.

(a) (Vc = 600 m/min, f = 0.1 mm/rev, ap = 3 mm). Wear is caused by the friction of the workpiece
on the flank face, the predominant wear is obtained under the effect of abrasion accompanied
by the wear caused by the migration of the substrate particles removed by the adherent chip.
Figure 12b shows for the conditions (Vc = 800 m/min, f = 0.1 mm/rev, ap = 3 mm), the chip
welding on the rake face has been abraded by rubbing on the workpiece surface. The chip
detachment will generate a catastrophic wear caused by the detachment of the substrate.
Figure 9c shows the conditions (Vc = 1000 m/min, f = 0.1 mm/rev, ap = 3 mm), we observe a

Figure 12. (a) 3D confocal image of the flank wear according (Vc = 600 m/min, f = 0.1 mm/rev, ap = 3 mm) for coating TiN
insert. (b) Confocal image of the flank wear according (Vc = 800 m/min, f = 0.1 mm/rev, ap = 3 mm) for coating TiN insert.
(c) 3D confocal image of the flank wear according (Vc = 1000 m/min, f = 0.1 mm/rev, ap = 3 mm) for coating TiN insert.
(d) 3D confocal image of the flank wear according (Vc = 1200 m/min, f = 0.1 mm/rev, ap = 3 mm) for coating TiN insert.
Dry High Speed Orthogonal Turning of Titanium Alloy Wear Evolution and Chip Morphology 77
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Figure 13. Orthogonal cutting zone. Zone 1 Primary shearing zone. Zone 2 Secondary shearing zone (interface friction
tool/chip). Zone 3 Tertiary friction (interface tool/workpiece zone).

flank wear caused by abrasion. Figure 9c shows a flank wear caused by high abrasion under
(Vc = 1000 m /min, f = 0.1 mm/rev, ap = 3 mm), conditions.

C. Chip morphology investigation

First investigations concerning the chip morphology obtained in very high speed orthogonal
turning by H13A uncoated and coated inserts tool material.

Using the optical microscope with high definition the Serrated chip obtained from experi-
ments is showing in Figure 13.

Geometry of the chip shape in these experiments was systematically investigated at each cut-
ting conditions using optical microscopy. The chips produced were collected and polished to

Figure 14. Serrated chip shape from experiments showing (a) shear zones, (b) the measured parameters [12].
78 Superalloys for Industry Applications

measure the thicknesses t2max and t2min, dch the distance between each segments and ɸseg the
inclination angle, see Figure 14. From t2max and t2min values, the degree of segmentation G was
evaluated by:

t −t
G = _______
2max
t
2min
(1)
2max

In high-speed machining the chip is segmented. The degree of segmentation gives an idea of
the shear rate. This quantity indicates whether or not the chip is forming well and that the
machining conditions are good.
Some pictures of serrated chips obtained for different cutting speeds, uncoated and coated
TiN carbide inserts are presented in Table 3 with 600 m/min cutting speed, and uncoated
insert we see the chip is segmented, but it is not uniform. For the cutting speed 800 m/min, the
chip is almost continuous, it is poorly segmented despite.

Significant strain in the shear zone. At the speed of 1000 m/min, the chip is uniform and well
segmented, machining conditions are favorable a 1200 m/min, the chip is segmented at the
beginning of machining, it is no longer uniform end machining (Figure 15).

As described in the introduction part, the shear angle ɸ and the inclination angle of a segment ɸseg
are differentiated as shown in (Figure 15). The angle ɸseg is actually measured on the collected
chips while the shear angle ɸ cannot be. The angle ɸ represents the initial shear similar to the one

Table 3. Photography of chip morphology.


Dry High Speed Orthogonal Turning of Titanium Alloy Wear Evolution and Chip Morphology 79
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Figure 15. Schematic diagram of the serrated chip [12].

that describes the formation of a continuous chip in the primary shear zone. Considering that an
element of volume, characterized by the angle ɸ, the length p and the width d is the source of a seg-
ment with the inclination ɸseg and the width dch, by applying the condition of incompressibility in
plastic deformation, we obtain the balance equation Finally, with the assumption that the values of
d and dch are close (d = dch), the initial shear angle f may be estimated by the following equation:

( (t 2max / cos ∅ seg) − d ch tan ∅ seg )
t1
∅ = arc 0sin ______________________ (2)

D. Analysis of the chip segmentation (Table 4)

Figure 16 shows that the degree of segmentation varies with the cutting speed. The largest value is
recorded for the speed Vc = 1000 m/min. as speed increases, the degree of segmentation decreases.
The variation of the degree of segmentation is more important for the TiN coated insert.

Figure 17 shows that the shear angle of the chip is larger for the coated insert. This value
decreases substantially at 1000 m/min cutting speed and then increases towards 1200 m/min.

Cutting speed m/min


Uncoated Coated Uncoated Coated Uncoated Coated Uncoated Coated

t2max 0.298 0.231 0.320 0.209 0.139 0.384 0.302 0.222

t2min 0.154 0.147 0.173 0.141 0.053 0.125 0.121 0.106

G 0.483 0.360 0.460 0.320 0.610 0.640 0.600 0.520

ɸseg 44° 73° 41° 37° 40° 59° 53° 59°

dch 0.111 0.088 0.111 0.078 0.056 0.181 0.112 0.070

Table 4. Parameters value of chip morphology.


80 Superalloys for Industry Applications

Figure 16. Degree of chip segmentation G evolution.

Figure 17. Evolution of shear angle ɸ.

Figure 18. Cutting force evolution according cutting speed for uncoating and TiN coating inserts.
Dry High Speed Orthogonal Turning of Titanium Alloy Wear Evolution and Chip Morphology 81
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E. Cutting force evolution

The cutting forces measured at the beginning of the cut for each condition are given in
Figure 18. Since the forces were measured at the beginning of the cut (first 5 s), it can be
assumed that tool wear is negligible and therefore, the observed cutting forces are a function
of the workpiece shear strength, chip shear angle and friction between the workpiece and tool.

Figure 18 shows the evolution of the cutting force Fc according to different cutting speeds.
For H13A insert the cutting force Fc did not increase significantly. For TiN coated insert the
cutting force Fc is important for cutting speeds (600 and 800 m/min), it greatly decreases in
the speeds range (1000/1200 m/min). We explained this by the fact for the uncoated H13A
plate there is no strong adhesion of the chip. For H13A coating TiN in cutting speed range
(600/800 m/min). There was a strong adhesion of the chip with the cutting face which gener-
ates a large friction. The high cutting speed facilitates the removal of the chip and reduces
adhesion. The cutting force is reduced.

4. Conclusion

Preliminary conclusion that can be given are:

At very high-speed machining of titanium alloy is possible. The detachment of the chip causes
it to migrate carbide grains.

The goal of this work was to propose a detailed analysis of geometry of the chip alloy Ti–6Al–4 V.

The originality of this approach lies in the speed range explored varying between 600 and
1200 m/min that corresponds for carbide tools to the field of high speed (500 m/min) and very
high speed (upper 600 m/min). This analysis helps to and proposes a hypothesis of their gen-
eration during high-speed machining. The ability to save snapshots of the cut in progress has
complemented the postmortem micrographic analysis of chips and strengthens the hypotheses.

Almost instantaneous increase temperature in the cutting area of the chip causes the welding
of the titanium alloy. The detachment of the chip causes it to migrate carbide grains.

In speed machining wear crater is the dominant wear on rake face and the final result is collapse
in cutting edge.

Microgeometry analysis of cutting edges is very important in the understanding of the chip
removal process. The interactions between the tool parameters, cutting parameters and the
effects on the machining procedure are all influenced and therefore determined by the peak
microgeometry. The evolution of the topography of crater wear using a confocal laser scanning
microscopy is a valuable tool for crater imaging. It provides more details than conventional
profilometers.

The chip formation of Ti-6Al-4 V alloy section is strongly influenced by crack initiation and
propagation, resulting in discontinuous or fragmentary morphology. When machining
Ti-6Al-4 V alloy at low cutting speed, the resulting chip is discontinuous, while at high cutting
speed, chip is serrated.
82 Superalloys for Industry Applications

Adhesion of the workpiece material occurs during titanium alloy machining, forming a BUE
along the cutting edge. This BUE modifies the geometry of cutting edge and, consequently, the
cutting forces. A better understanding of the relationship between cutting forces and both the
shape and the size of the BUE must be realized in the future. It might be interesting to carry out
tests with higher feed rates (by example 0.2 mm−1). In terms of chip formation we notice adia-
batic shear even at the lowest cutting speeds. This phenomenon is typical of titanium alloys.
To reduce wear, we must develop a system of lubrication located using the MQL technique.

Find a hard coating that will oppose the chip welding titanium alloy with the substrate of the
insert. Why you should test other types of diamond coating for example.

Develop cryogenic lubrication to prevent heating in the cutting area.

Author details

Mohieddine Benghersallah1*, Lakhdar Boulanouar1, Gautier List2 and Guy Sutter2


*Address all correspondence to: bengher_moh@yahoo.fr
1 Research Laboratory in Advanced Technology and Mechanical Production, Department of
Mechanical Engineering, Badji Mokhtar Annaba University, Annaba, Algeria
2 LEM3, UMR 7239, Université de Lorraine – Ile du Saulcy, Metz Cedex, France

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DOI: 10.5772/intechopen.76347

Provisional chapter
Chapter 6

Laser
Laser Welding
Welding of
of Different
Different Dental
Dental Alloys
Alloys

Lavinia
Lavinia Cosmina Ardelean, Lucien Reclaru,
Cosmina Ardelean, Lucien Reclaru,
Cristina Maria Bortun
Maria Bortun and Brandusa Ghiban
Brandusa Ghiban

Additional information is
Additional information is available
available at
at the
the end
end of
of the
the chapter
chapter

http://dx.doi.org/10.5772/intechopen.76347

Abstract

Laser welding permits joining various types of pieces, made of similar or different alloys,
as titanium-based alloys, CoCr alloys, and even AuPd alloys. Laser welding is best suited
to weld titanium alloys because they have higher rates of laser beam absorption and
lower thermal conductivity compared to other dental casting alloys. Compared to micro
pulse welding, laser welding is superior, obtaining the welding cord being faster and
easier. The success of the welding procedure depends on the operator’s dexterity and the
choice of the welding parameters. Selecting the best combination of pulse energy, pulse
duration, and peak power for each welding step is decisive.

Keywords: laser welding, micro pulse welding, dental alloys, welding assessment,
welding cord

1. Introduction

Welding in dentistry involves small metallic areas, often in the proximity of resin or ceramic
structures, which may be damaged by heat (Figure 1). The fracture of a metallic frame usu-
ally happens in an area of minimum resistance. This type of damage could not be repaired
15–20 years ago, using welding systems available at that time.

Nowadays, two types of welding are suitable for use in dental technique: laser and micro
pulse [1].

After Nd:YAG lasers appeared in Europe, in 1990, laser welding has been extended to dental
technique and permits joining various types of pieces, which might have been difficult or even
impossible to do with other techniques.

© 2016 The Author(s). Licensee InTech. This chapter is distributed under the terms of the Creative Commons
© 2018 The Author(s). Licensee IntechOpen. This chapter is distributed under the terms of the Creative
Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use,
Commons Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use,
distribution, and reproduction in any medium, provided the original work is properly cited.
distribution, and reproduction in any medium, provided the original work is properly cited.
86 Superalloys for Industry Applications

Figure 1. Laser welding of a fractured clasp and frame.

Figure 2. Welded CrNi stainless steel orthodontic ring and wire.

It permits joining similar or different alloys, as titanium-based alloys, CoCr alloys, and even
AuPd or CrNi stainless steel alloys (Figure 2).
In laser welding, heating and melting are limited to a small area, which prevents damaging
the components of the denture pieces which might deteriorate when heated (resins, ceramics)
(Figure 3). It permits the welding of elements situated in places difficult to reach, such as the
inner parts or extremely small, delicate, and sensible elements. It is very efficient in repairing
the framework of removable partial dentures, being fast, economic, and very accurate [2].

It may also be used for manufacturing removable partial dentures, by joining pieces which
might be difficult to cast in one piece, due to various reasons, such as high contraction at cast-
ing. One of the main advantages of the method is that of “cold” welding, on a model or even
in hand. Nowadays even “in-mouth welding” is possible [3].

All laser welding devices used in dental technique are equipped with an optic enlarging sys-
tem which permits perfect visualization of the fragments to be welded (Figure 4), the space
between them, and the position of the filler metal, when used. The filler metal (special wire
for laser welding) is the same type as the base material and has to be used when there is some
space between the two pieces to be welded. Welding without a filler material may be carried
out when the distance between the two pieces to be welded is almost imperceptible [4].
Laser Welding of Different Dental Alloys 87
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Figure 3. Welding of a fractured clasp in close proximity to the saddle made of an acrylic resin.

Figure 4. XXS laser welder for dentistry (Orotig) and its enlargement system.

Laser welding in dental technique often uses a protected environment, argon 4.6 with a purity of
99.996% or argon 5.0 with a purity of 99.999%, in order to prevent the oxidation of the alloys [4].

Laser welding may be done in continuous or pulsed mode. The parameters which may
be modified in case of welding with a Nd:YAG laser, in a continuous emission mode, are
the radiation power, the welding speed, and the diameter of the laser beam. The radiation
power variation is limited by the manufacturer and does not have a great influence on the
welding depth. The diameter variation of the laser beam is also limited, in order to obtain
the minimum density of the energetic wave; consequently, the only parameter which may
significantly influence the morphology of the welding is the welding speed. A low welding
speed does not necessarily imply a greater welding depth. In case of noble alloys, optimal
welding speed is considered to be 10.1 cm/min, and it doubles in the case of base metal
alloys: 20–25 cm/min. These parameters permit a welding depth of 0.8 mm for noble alloys
and up to 2.0 mm for base metal alloys. Variations by 20% of these parameters may lead to
incomplete welding (too high speed) or uncontrolled melting, which may compromise the
entire piece [4].
In case of Nd:YAG laser welding pulsed mode, the density of the energetic flux is at least 10
billion times greater than when using the continuous mode. The exposure time is very short,
so the thermal conductivity of the alloy is of less importance. In this case, the morphology of
88 Superalloys for Industry Applications

the welding is influenced by the impulse energy, length, and frequency. In case of high energy
density, the side effects which appear in the welded structure may not be generalized [4].

The action of the laser beam that leads to the formation of the welding cord can be described
as follows (Figure 5):

• The material is first heated by conduction.

• The absorbed energy superficially penetrates the alloy, melting the impact surface.

• A metallic vapor develops in the center of the impact point. The material partly absorbs
and diffuses the energy of the beam.
• The vapor pressure increases and dispels the melting alloy to the periphery of the beam and
upward. This results in creating a narrow (capillary) shaft which propagates through the ma-
terial. This shaft, with a diameter barely greater than the beam, is physically filled by metallic
vapor plasma. Its walls are coated with a film of melting metal maintained by capillarity.

• The melting metal is finally sent backward and closes the welding cord (Figure 6) [5, 6].

The quality of micro pulse welding is comparable to that of laser welding. It has the advantage
of a lower initial investment, but it uses electrodes that are consumed in time and have to be
replaced. When compared to laser welding, micro pulse welding appears to be more visible
and embossed (Figures 7 and 8). The probability of developing pores is higher, compared to
laser welding, which is much more compact [7].
Welding in dental laboratories is made by melting small surfaces of the metallic piece. Each
time, a welding cord with overlapped spots will be obtained (Figure 6). The area in close
proximity, named thermally affected area (TAA), is very sensitive to thermal variations after
welding, as sudden cooling of the material, which might lead to cracks. The TAA is usually
tougher than the base material (BAA), from which the welded piece is manufactured.

The quality of the welding depends on the alloy’s nature, the welding mode, and the laser’s
parameters [4].

Figure 5. Stages of the welding cord formation.


Laser Welding of Different Dental Alloys 89
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Figure 6. (a) Image of the welding cord. (b) Microscopic image of the welding points.

Figure 7. Micro pulse welded piece.

Figure 8. Appearance of micro pulse welding (a) compared to laser welding (b).

The quality of laser welded joints for different dental alloys may be evaluated by different
invasive methods, metallographic analyses and microhardness testing, and noninvasive
methods, dye staining, X-ray, and microscopy [8, 9].

2. Welding of TA6V4 and AuPd alloys

The TA6V4 alloy is a titanium-based alloy containing 6% aluminum and 4% vanadium,


mainly used in manufacturing ready-made pieces for implantology.
90 Superalloys for Industry Applications

Figure 9. Schematic pseudo-binary phase diagram of TA6V4 alloy.

The alloy is biphased Tiα + Tiβ, at room temperature, with a slight phase percentage for Tiβ,
as shown in the pseudo-binary phase diagram (Figure 9). The existence of the two phases Tiα
and Tiβ, at room temperature, enables creating an alloy with a high mechanical resistance,
due to the mutual interaction of the two phases. The alloy has an elasticity limit of 875 MPa.
During heating, the Tiα turns into Tiβ at approximately 980°C. During fast cooling, the Tiβ
phase undergoes a so-called martensitic transformation forming a complex lamellar struc-
ture inducing significantly altered mechanical properties. These mechanical properties will
be recovered by a low-temperature thermal treatment.

This alloy welds mainly to itself or to other alloys by laser welding. Metallurgic analysis, by
metallography and scanning electron microscope (SEM) observation, after a single impulse

Figure 10. Schematic description of the cord during welding.


Laser Welding of Different Dental Alloys 91
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Figure 11. SEM observation of the TA6V4 cord sample after a single impulse laser impact.

laser impact, of the sample is characterized (Figures 10 and 11) in the following way: after
cooling, there is a melting area (MA), a thermally affected area (TAA), and an area corre-
sponding to the base alloy (BAA) [10].

• The MA is mainly formed of Tiα turned by martensitic transformation into Tiα’.


• The TAA is mainly composed of two sublayers developed in the proximity of MA, formed
of a Ti″ structure and, deeper down, of a complex Tiα + Tiα + Tiα’ structure.

• The BAA consists of the Tiα + Tiβ structure.

The AuPd alloy welded by laser technique is the standard Qualibond 2 (PX Dental/Qualident)
alloy for the metallo-ceramic technique, containing 51.2% Au, 38.6% Pd, indium, gallium, and
ruthenium as additional elements.
For the AuPd alloy for the metallo-ceramic technique, Figure 12 shows the successive impacts
leading to the welding of the two pieces. Like in the case of a titanium-based alloy, there is a
very perturbed TAA (Figure 13) and a lamellar structure of the MA (Figure 14).
In case of TA6V4 alloy, the cooling speed plays an important role on the mechanical charac-
teristics due to its influence on the phase transformation structures into a solid state. The elasti-
city limit during high temperatures decreases, and the resistance to wear is rather unaffected by
laser welding due to the fact that the cord has no porosities or other defects (cracks, snaps) [11].
In case of the AuPd alloy for the metallo-ceramic technique, it appears the fracture toughness
of the laser welded area is higher than in the case of brazing. On the other hand, the wear
resistance of the laser welding is lower than in the case of brazing (Figure 15).
The quality of the welding is mechanically satisfactory. In order to avoid problems, initially,
both parts of the joined piece should be subjected to low-level energy impacts, followed by
greater energy for filling. The success of the welding procedure also depends on the opera-
tor’s dexterity and the choice of the welding parameters [12].
92 Superalloys for Industry Applications

Figure 12. Welded area (SEM).

Figure 13. MA, TAA, BAA areas (metallography).

Figure 14. MA area (metallography).


Laser Welding of Different Dental Alloys 93
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Figure 15. (a) Fracture toughness (MPa). (b) Resistance to wear (MPa).

3. Welding of three different CoCr alloys

Three different CoCr alloys, frequently used for manufacturing metallic frameworks of
removable partial dentures, were tested: Heraenium CE (Heraeus Kulzer), Wironit Extra-
Hard (Bego), and “C” alloy (Vaskut Kohàszati Kft). The chemical composition and mechanical
properties of the alloys are shown in Table 1.
The alloys were analyzed both in the form of metallic frameworks of removable partial den-
tures (Figure 16) and as metallic casted plates with dimensions 10x20mm and thickness of
0.4 mm (Figure 17). For improving the structure of the alloy plates, heat treatments at differ-
ent temperatures were applied.
In some cases, the use of a filler metal, special 0.5 mm diameter CoCr Finalloy filler (Fino), was
needed (Figures 18 and 19).
The equipment used for welding consisted of Welder micro pulse (Schütz Dental) and Laser
65 L-Titec (Figure 20).
Welded joint quality was tested by radiographic, microscopic, metallographic, and micro-
hardness tests [13].
In order to assess the quality of the welded joints and visualize possible structural defects as
cracks in the base materials, X-rays and microhardness tests were carried out. The inverted

Tested alloys Co Cr Mo Si Mn C Tensile strength Rm Vickers hardness


Heraenium CE 63.5 27.8 6.6 1.0 0.6 — 890 N/mm 2
380 HV

Wironit Extra-Hard 63.0 30.0 5.0 1.0 1.0 <1.0 910 N/mm 2
385 HV

”C″ alloy 65.0 29.0 5.0 0.35 5.0 0.4 760 N/mm 2
380 HV

Table 1. The chemical composition and mechanical properties of the three alloys.
94 Superalloys for Industry Applications

Figure 16. Some fractured metallic frameworks of removable partial dentures, before and after welding.

metallurgical microscope and the stereomicroscope enabled the observation of different pro-
cessing aspects of the metallic components, relevant for the welding procedure.
Microhardness analysis was carried out using a 100 g charge, five to six impressions for each
area of the welded joint being made, and shows a small increase of the hardness in TAA and
Laser Welding of Different Dental Alloys 95
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Figure 17. (a) The casted plates. (b) Plates after welding.

MA. The hardness in the MA shows values between those of the BAA and TAA. Microhardness
values of the welded joints are up to 15% lower in the TAA for Wironit Extra-Hard (Bego),
with no heat treatment, and higher up to 16% if heat treatment was made.

In case of Heraenium CE (Heraeus Kulzer) microhardness, part of the samples without heat
treatment shows no changes in the MA and TAA; part of the samples shows decreased values
up to 25%. Samples which had undergone heat treatment show no changes.

In case of “C” alloy (Vaskut Kohàszati Kft), part of the samples shows no microhardness
changes; part of the samples shows decreased values up to 33%.

These values are of no great importance as microhardness variations may appear due to lack
of homogeneity of the casted base alloy [14].

X-rays show casting defects, such as lack of material and cracks within the base material
(BAA). A radiotransparency on the welding line and some imperfections in the clasps welding
area may be observed (Figure 21).

For the “C” alloy (Vaskut Kohàszati Kft), the welding area, dyed in yellow, shows no fis-
sures in the immediate vicinity of the welding, in the TAA, because the laser was used at
very low temperatures and there are no contractions in the analyzed material. However,
X-rays show radiotransparency in the MA, which indicates a superficial fusion which does
not cover the entire thickness of the plate. (Figure 22) Despite the fact that the plates used
are not very thick, welding does not cover the whole depth. This results in the fragility of
the welding [11, 13].

Microstructural analysis presents the relative homogeneous dendritic structure specific for
casted alloys, nonmetallic inclusions, and some chemical compounds. Intergranular pre-
cipitations and spherical shape compounds, consisting of alloy’s elements, placed inside
96 Superalloys for Industry Applications

Figure 18. Laser welding without filler metal.

Figure 19. Laser welding with filler metal.


Laser Welding of Different Dental Alloys 97
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Figure 20. The micro pulse welding device Welder (Schütz dental) and laser 65 L-Titec with welding parameters.

Figure 21. Radiographic images: (a) Metallic framework. (b) Welded plates.

Figure 22. Assessment of the welded “C” alloy (Vaskut Kohàszati Kft) area: (a) Basic fuchsin dye staining. (b) X-ray
pseudo-chromatization.
98 Superalloys for Industry Applications

Figure 23. Microcracks in the BAA dendritic structure spread along the fragile compound precipitations, in case of fast
cooling of the welded alloy.

Figure 24. (a) Nonuniform dendritic structure with interdendritic cracks and microporosities. (b) Microstructural aspect
of the welding cord in case of “C” alloy (Vaskut Kohàszati Kft), with cracks due to laser exposure, spreading from
surface to center.

the crystalline grains with well-delimitated boundary limits, which are characteristic to the
solidification process, appear in case of some welded joints (Figures 23, 24, and 25). This may
often lead to alloy durification and fragile structure.

Metallographic analysis of the laser welded joints is shown in Figures 26, 27, and 28.

Figure 29 shows pellicular intergrain precipitations and spherical shape compounds, placed
inside the crystalline grains.

Metallographic analysis indicates that welded CoCr alloys exhibit rather large microstruc-
tural defects, including interdendritic carbide precipitations, segregation, relatively large
grains, and porosity, mainly in the BAA area. These microstructural defects may lead to crack
initiation. The welded joints themselves (MA) show a rather good quality.
Laser Welding of Different Dental Alloys 99
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Figure 25. Wironit extra-hard (Bego) sample. (a) Welded on both sides, with nonuniform dendritic structure. (b) With
thermal treatment, with nonuniform fine dendritic structure and carbide inclusions.

Figure 26. Microstructural aspect of Heraenium CE (Heraeus Kulzer). (a) Laser welded samples MA and TAA,
microhardness values unchanged. (b) Laser welded samples without thermic treatment, MA microhardness values
decreased up to 25%. (c) Micro pulse welded samples, heat treated, no microhardness changes in the TAA.

Figure 27. Microstructural aspect of Wironit extra-hard (Bego) laser welded samples. (a) TAA microhardness values
lower up to 15%. (b) Samples with heat treatment, TAA microhardness values higher up to 16%.

Noninvasive analysis points out the structural defects of the three casted alloys, showing
cracks which grow proportionally with the thickness of the alloy, within the BAA. These may
be caused by casting, improper processing, and rapid cooling after welding [15, 16].
100 Superalloys for Industry Applications

Figure 28. Microstructural aspect of “C” alloy (Vaskut Kohàszati Kft) laser welded samples. (a) TAA microhardness
values lower up to 30%. (b) TAA microhardness values unchanged.

Figure 29. Metallographic aspects of pellicular intergrain precipitations, spherical shape compounds.

Figure 30. Microscopic aspects of Wironit extra-hard (Bego) alloy for different laser beam sizes: (a) small, (b) medium,
(c) large.
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Figure 31. Microscopic aspects of “C” alloy (Vaskut Kohàszati Kft) for different laser beam sizes: (a) small, (b) medium,
(c) large.

The welding defects (cracks) appear to be in connection with the laser beam size and laser
power. Most of the cracks appear at big spot/ high power association, during the welding
smoothing (Figures 30 and 31) [17].

4. Welding complex CoCrMoTi(Zr) alloys

Welding experiments on complex CoCrMoTi(Zr) alloys, CoCrMoZrTi alloy, CoCrMoTi4 alloy,


and CoCrMoTi5.5 alloy [18–24], were performed by selecting three categories of parameters,
a selection which was made following previous tests on cobalt alloys. For this purpose, the
welding parameters were chosen, with three values of the laser spot power, namely, low
power (1.9 W), average power (2.0 W), and higher power (2.3 W); the times of application of
the spot, namely, short (1.1 s) or long (1.3 s); and the frequency of the spot application at two
levels, respectively, 2.0 Hz and 3.0 Hz. (Table 2).
The macrostructural analysis carried out on the welded surfaces of the complex
CoCrMoTi(Zr) alloys is shown in Figures 32–34. This analysis proved to be decisive in
the selection of welding parameters as it allowed to highlight these parameters correlated
with the macrostructural aspect. Thus, in the case of the first set of welding parameter
values, all alloys presented similar macrostructural aspects, consisting of non-cracked
welded cords. The second set of values resulted in partially satisfactory results, with all
alloys presenting a nonconforming welded surface. Regarding the third set of welding
values, it led to the most inappropriate results. Thus, in all alloys, the high value of the
welding spot power generated the subsequent melting of the welding cord, due to the
generation of sprays from the next step. It can be said that the welding performed with

Parameter Power Time Frequency


Set 1 2.0 W 1.1 s 2.0 Hz
Set 2 1.9 W 1.3 s 3.0 Hz
Set 3 2.3 W 1.3 s 2.0 Hz

Table 2. Sets of parameters used for welding CoCrMoTi(Zr) alloys.


102 Superalloys for Industry Applications

Figure 32. Macroscopic aspect of the welded CoCrMoZrTi alloy using different parameter values: (a) first set, (b) second
set, (c) third set.

Figure 33. Macroscopic aspect of the welded CoCrMoTi4 alloy using different parameter values: (a) first set, (b) second
set, (c) third set.

Figure 34. Macroscopic aspect of the welded CoCrMoT5.5 alloy using different parameter values: (a) first set, (b) second
set, (c) third set.

the parameters corresponding to the first set of values generates the best quality weld-
ing cord, without the presence of cracks. The microstructural analysis (Figures 35–37)
confirms the macrostructural one. In the case of the first set of welding parameters,
no cracks were observed either in the welding cord or TAA in all alloys, irrespective
of the thermal treatment state (Figure 35a, 36a, and 37a). In the case of the second set of
values, the presence of cracks generated either on the welding cord and developed in the
TAA (as for the CoCrMoZrTi alloy), or strong cracks in the center of the welding cord
(CoCrMoTi4 alloy, CoCrMoTi5.5) are present. Similar observations were also recorded on
Laser Welding of Different Dental Alloys 103
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Figure 35. Microscopic aspect of the welded CoCrMoZrTi alloy using different parameter values: (a) first set, (b) second
set, (c) third set.

Figure 36. Microscopic aspect of the welded CoCrMoTi4 alloy using different parameter values: (a) first set, (b) second
set, (c) third set.

Figure 37. Microscopic aspect of the welded CoCrMoT5.5 alloy using different parameter values: (a) first set, (b) second
set, (c) third set.

samples welded using the third set of parameters, the difference being the dimensions and
the crack propagation. Thus, in the case of the third set of welding parameters, larger cracks
with transgranular propagation may be noticed in almost all situations.

5. Discussions

Laser and micro pulse welding is mainly used in dentistry for repairing damaged metallic
parts of partial dentures or orthodontic appliances [25].
104 Superalloys for Industry Applications

If welding is used for repairing or completing damaged areas of prosthetic pieces, struc-
tural modifications are expected, especially in TAA, regardless of the welding type. In this
area, due to overheating and fast cooling, precipitates of certain alloy chemical compounds
may appear. These precipitates increase the hardness of the welded metal and lead to fragile
areas, which could crack during functional loads. Cracks may appear not only because of the
mechanical stress to which the dentures are exposed but also during manufacturing stages
and may lead to fracture. Thermal treatments improve the structure and quality of the casted
and welded alloys [4].

In order to obtain dentures with good resistance, it is very important to assess the quality and
potential structural defects of the welded parts.

The success of the welding procedure depends on the operator’s dexterity and the choice of
the welding parameters. Selecting the best combination of pulse energy, pulse duration, and
peak power for each welding step is decisive [20, 24].

Laser welding is best suitable to weld titanium and its alloys because they have higher rates
of laser beam absorption and lower thermal conductivity compared to other dental casting
alloys such as gold or CoCr alloys; however, due to the strong reactivity of molten titanium
with oxygen in ambient air, the incorporation of oxygen during laser welding may affect the
joint strength.

The initial welding is carried out by using a small laser beam (which better penetrates the
alloy); afterward, a large beam is used for surface smoothening. Optional welding may be
carried out in argon protective environment. The pulsed mode is preferred.

In the case of base metal alloys, the beam diameter must not be smaller than 1.5 mm, a 0.8 mm
depth being considered enough to obtain a good breaking resistance. In case of heavy loads,
both sides of the defect are welded.

Welding without filler metal is very scrupulous and implies a perfect surface processing and
a uniform proximity of maximum 0.1 mm (which enables a good welding resistance), which
is difficult to obtain in daily practice. Furthermore, the penetration depth and the metallo-
graphic changes in the TAA are difficult to manage. From this point of view, welding with
filler metal is better, because the breaking resistance is reproducible, welding being carried
out by conducting heat along the interfaces.

Welded alloys without carbon act better than those which have carbon in their composition.
During welding, excess carbide precipitations may occur, which leads to hardening (fragiliza-
tion) of the TAA and possible cracks.

In case of repairs, an important element is determining the initial cause of the fracture. If it’s
the consequence of a casting or conception mistake, the welding will not last for long.

With a proper selection of laser parameters for welding, one may obtain very good welded
pieces, with no cracks (as showed in our experiments carried on CoCrMoTi(Zr) system
alloys).
Laser Welding of Different Dental Alloys 105
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6. Conclusions

The advantages of laser welding in dental laboratories may be summarized as follows: it is


time-saving; potentially all types of metals may be joined, particularly titanium alloys; welds
are made on the model, distortions being avoided; the absence of corrosion, because no sol-
dering alloy is needed; good resistance of the welded area; and the possibility to weld in
proximity of resins or ceramic materials without damage.

Compared to micro pulse welding, which needs the use of a changeable electrode, laser weld-
ing is superior, achieving the welding cord being faster and easier in case of laser welding.

Author details

Lavinia Cosmina Ardelean1*, Lucien Reclaru2, Cristina Maria Bortun3 and Brandusa Ghiban4
*Address all correspondence to: lavinia_ardelean@umft.ro
1 Department of Technology of Materials and Devices in Dental Medicine, “Victor Babes”
University of Medicine and Pharmacy, Timisoara, Romania
2 Consultant, Corrosion and Biocompatibility Department, VVSA, Branch of Richemont
International SA Varinor Innovation, Switzerland
3 Department of Dentures Technology, “Victor Babes” University of Medicine and
Pharmacy, Timisoara, Romania
4 Department of Metallic Materials Science, Physical Metallurgy, Faculty of Science and
Engineering of Materials, “Politehnica” University of Bucharest, Romania

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Edited by Sinem Cevik
In recent years, superalloys have been widespread usage in aerospace gas turbine engine
parts. The main reason of it is that these materials have high yield, ultimate tensile strength,
and very good corrosion/oxidation resistance, and they combine these good properties
with an excellent creep resistance at elevated temperatures. In spite of their outstanding
properties, superalloys can lose their mechanical strength because of wear, tear, and
crack formation when they are exposed to high-service temperatures and heavy working
conditions. Moreover, corrosion is another important issue for superalloys because the
materials of gas turbine engine parts are exposed to harsh engine environments, which
consist of many pollutants and hot gases. Therefore, special attention must be given to the
corrosion behavior of superalloys.
This book provides information on the interaction between the microstructure of alloys
and their mechanical properties and also the position of superalloys in the manufacturing
industry. Topics cover the minimization of the formation of microsegregation and
detrimental phases in the GTA welding of superalloys, oxidation kinetics of nickel-based
superalloys used in the manufacture of rings for aircraft engines, a review of the work done
over the last two decades to understand the hot corrosion behavior of superalloys used in
advanced coal-based power plants, ultrasonic-assisted machining of Inconel 718, dry high-
speed turning of Ti-6Al-4V titanium alloy, and laser welding in dentistry.
The book “Superalloys for Industry Applications” consists of contributions by scientists and
engineers who are experienced in the production, design, and analysis of materials from
all around the world. We hope that this book will be an irreplaceable source of study for
manufacturing, degradation mechanisms, and reliability of superalloys.

ISBN 978-1-78923-539-5
978-1-78923-538-8

Published in London, UK
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